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温医大项目汇总表-温州医科大学附属第二医院
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温医大项目汇总表-温州医科大学附属第二医院
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3秒自动关闭窗口请教大神移植五个月，他克莫司浓度6.5是否合适医生也没加药。_移植吧_百度贴吧
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请教大神移植五个月，他克莫司浓度6.5是否合适医生也没加药。收藏
请教大神移植五个月，他克莫司浓度6.5是否合适医生也没加药。
肌酐稳定就可以呗。
低了 应该7-9
非常好，我两月6医生都没加药，还只吃2mg
现在4月涨到7，没法减了，一天总共才2mg
查个T淋巴细胞亚群，大部分移植肾慢排都是浓度低引起的
6.5很好啊，我四月医生建议4-7，个人感觉内地医院浓度普遍偏高，沿海医院都偏低，我浙江的，在郑州手术，郑州医生建议6-9，还是相信沪浙医院
这个浓度如果是在浙一医院的话，不要太好的。其他医院就不太了解了，像这样的浓度根本用不着调药的。
北京武总标准，起始才6-8,保持半年，他们的理念是防感染优先排异，当然这边配型很严格，外腎没三个大点不做
我浓度9.2,减药了
我老公今天刚去查了他克莫司的浓度，刚移植2个月，浓度6，我们在温州复查的，医生说高了，减量，我们手术是在武汉中南做的，浓度一直保持在7.3左右，浓度太低是不是肌酐也降不下来啊
登录百度帐号推荐应用药物分析杂志Chin J Pharm Anal )摘要
内容模板2007
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药物分析杂志Chin J Pharm Anal )摘要
纳升电喷雾串联质谱鉴定吗啡依赖2个重要相关蛋白的N端乙酰化修饰
国家863计划资助项目(No.)和973计划资助项目()
何家田1，刘炳玉1，吴宁2，苏瑞斌2，李锦2，张学敏1，魏开华1，王红霞1
（1.国家生物医学分析中心，北京 100850；2.军事医学科学院毒物药物研究所，北京 100850）
摘要 目的：用纳升电喷雾串联质谱(nanoESI-MS/MS)鉴定吗啡依赖相关蛋白。方法：采用吗啡递增给药法建立吗啡依赖模型，用纳洛酮催促后出现典型的戒断症状，以盐水组为对照，对长期接受吗啡处理和纳洛酮催促戒断这2种状态的大鼠纹状体进行了比较蛋白质组研究，确定了33个差异点。其中差异点150和209用电喷雾串联质谱进行了氨基酸序列分析。结果：电喷雾串联质谱分析表明差异点150和209为2个重要的吗啡依赖蛋白质：G蛋白β1亚基和电压依赖型阴离子通道蛋白1（VDAC-1），并且这2个蛋白质都发生了N端乙酰化修饰。结论：纳升电喷雾串联质谱分析是研究蛋白质N端乙酰化的好方法。N端乙酰化对蛋白质生物学功能有重要作用。这2个蛋白质N端乙酰化的生物学功能及其与吗啡依赖的关系值得深入研究。
关键词：吗啡依赖；乙酰化；G蛋白β1亚基；电压依赖型阴离子通道蛋白1（VDAC-1）；纳升电喷雾串联质谱(nanoESI-MS/MS
中图分类号：R917&&&& 文献标识码：A&&&&& 文章编号：08)02-0171-05
Characterization of N-terminal acetylation of two morphine
dependence related proteins with nanoESI-MS/MS*
HE Jia-tian1,LIU Bing-yu1,WU Ning2,SU Rui-bin2,LI Jin2,ZHANG Xue-min1,WEI Kai-hua1，WANG Hong-xia1**
（1.National Center of Biomedical Analysis,Beijing 100850,China;
&&&&&&&&&&&&&&&&&&&& 2.Beijing Institute of Pharmacology and Toxicology,Beijing 100850,China)
Abstract Objective:To characterize morphine dependence differential proteins by nano electrospray tandem mass spectrometry (nanoESI-MS/MS).Method:The rats were treated with ascending doses of morphine to achieve dependence and leading to characteristic withdrawal syndromes after naloxone-parative proteomic analysis was performed in striatum of two phases of morphine dependence,long-term exposure to morphine and drug withdrawal and 33 different protein spots were identified by matrix-assisted laser desorption/ionization-time-of-flight-mass spectrometry (MALDI-TOF-MS).The differential spot 150 and 209 were analyzed by nanoESI-MS/MS since they were not identified by MALDI-TOF-MS unambiguously.Results:NanoESI-MS/MS analysis indicated that spot 150 and 209 were G protein β1 subunit and voltage-dependent anion-selective channel protein 1 (VDAC-1) respectively.Most importantly,nanoESI-MS/MS analysis showed that the two proteins are all N-terminally acetylated.Conclusion:NanoESI-MS/MS is a powerful tool for N-terminal acetylation analysis.N-terminal acetylation &is critical to biological function of proteins.It is worth of giving insight into function of the two N-terminal acetylated proteins and their relations to morphine dependence.
Key words:G protein β1voltage-dependent anion-selective channel protein 1;nano electrospray tandem mass spectrometry(nanoESI-MS/MS)
吉九里香碱体外诱导HCT-15细胞凋亡的研究
国家重点基础研究发展规划项目（973项目）基金（No.）；国家杰出青年基金（No.）
第一作者Tel:(010)；Fax：(010)；E-mail：
王三龙1，蔡兵2，崔承彬3，阎少羽4，吴春福4
（1.中国药品生物制品检定所国家药物安全评价监测中心，北京 100176；2.北京生物医药研究所，北京 100091；
3.北京药理毒理研究所，北京 100850；4.沈阳药科大学中药学院药理系，沈阳 110016）
摘要 目的：探讨中药单体吉九里香碱是否通过诱导HCT-15细胞凋亡而发挥其抑制肿瘤细胞增殖的作用。方法：采用MTT法检测细胞增殖抑制作用；采用透射电子显微镜观察细胞凋亡的形态学变化；库尔特全自动颗粒粒度分析药物引起HCT-15细胞体积大小分布的变化；琼脂糖凝胶电泳测定DNA ladder的发生；通过流式细胞仪应用Annexin V-FITC和Rhodamine123检测磷脂酰丝氨酸（PS）及线粒体跨膜电位（△ψm）。结果：MTT结果显示吉九里香碱以浓度和时间依赖方式抑制HCT-15细胞的增殖，抑制率依赖于吉九里香碱的浓度和作用时间；50 μmol?L-1吉九里香碱处理HCT-15细胞24 h时，细胞出现凋亡典型的形态学特征；50 μmol?L-1吉九里香碱分别处理HCT-15细胞6，12，24 h及不同浓度吉九里香碱处理HCT-15细胞24 h时，能够使细胞产生明显的DNA ladder和体积大小变化，呈一定的量效和时效关系；细胞PS外翻随作用时间的延长而增加，分别为15.34%（6 h），20.20%（12 h），39.37%（24 h）；50 μmol?L-1吉九里香碱处理HCT-15细胞导致线粒体△ψm以时间依赖方式下降。结论：吉九里香碱通过诱导HCT-15细胞凋亡而发挥其抗HCT-15细胞增殖的作用，致凋亡机理可能与线粒体△ψm快速下降有关。
关键词：细胞凋亡；HCT-15细胞；黑果黄皮；吉九里香碱
中图分类号：R917&&& 文献标识码：A&&& 文章编号：08)02-0176-06
Study on induction of apoptosis by girinimbine in HCT-15 cell in vitro*
WANG San-long1,CAI Bing2,CUI Cheng-bin3,YAN Shao-yu4,WU Chun-fu4
(1.National Center for Safety Evaluation of Drugs,National Institute for the Control of Pharmaceutical & Biological Products,Beijing .Beijing Institute of Biomedicine,Beijing .Beijing Institute of Pharmacology and Toxicology,Beijing .Department of Pharmacology,School of Chinese Material Medica,Shenyang Pharmaceutical University,Shenyang 110016,China)
Abstract Objective:To investigate if girinimbine inhibits the proliferation of HCT-15 by inducing its apoptosis.Methods:Cell proliferation inhibition was assessed by MTTMorphological changes of apoptosis were observed with invert fluThe distribution of the cell volume sizes was assessed by Coulter Multisizer Ⅱ aDNA ladder was examined by DNA agarosePhospholipid phosphatidylserine (PS) and mitochondrial transmembrane potential(△ψm) were measured with Annexin V-FITC and fluorescent probe Rh123,respectively.Results:MTT assay showed that girinimbine inhibited the proliferation of HCT-15 cells in a time-and concentration-dependent manner.HCT-15 cells treated with 50 μmol?L-1 girinimbine for 24 hours showed typical morphological changes of apoptotic phase.After treated with 50 μmol?L-1 girinimbine for 6,12 and 24 hours or with girinimbine in different concentrations for 24 hours,respectively,there were obvious changes of DNA ladder and the distribution of the cell volume size.The results obtained with Annexin V-FITC kit showed that the percentage of the apoptotic cells was 15.34% (6 h),20.20% (12 h),and 39.37% (24 h).The treatment with 50 μmol?L-1 girinimbine resulted in a rapid decrease of △ψm in a time-dependent manner.Conclusion:These results suggest that girinimbine shows its anticancer activity by inducing apoptosis of HCT-15 cells,and its apoptosis inducing mechanism may involve the rapid decrease of △ψm.
Key words:apoptosis;HCT-15Clausena dunniana Levl.;girinimbine
栀子苷和4种黄酮类成分的含量
邓远雄1，2，刘李1，俞森1，谢林1，刘晓东1
通讯作者Tel:(025);E-mail:
(1.中国药科大学药代动力学重点实验室，南京 210009；2.湖南师范大学医学院，长沙 410006)
摘要 目的：建立一种同时检测黄连解毒汤中栀子苷、黄芩苷、汉黄芩苷、黄芩素和汉黄芩素含量的HPLC方法。方法：采用Kromasil C18 色谱柱(150 mm×4.6 mm,5 μm)，以乙腈(A)-5 mmol?L-1磷酸二氢钠溶液(含0.05%磷酸,pH 3.0)(B)为流动相，线性梯度洗脱(0~8.5 min,86.5%B；8.5~17.0 min,86.5%B→80%B；17~30 min,80%B；30~40 min,80%B→60%B；40~51 min,60%B→52%B；51~55 min,52%B→42%B；55~60 min,42%B→86.5%B；60~65 min,86.5%B)，流速1.0 mL?min-1，程序可变波长紫外检测(0~15 min,23815~50 min,276 nm)。结果：在58 min内黄连解毒汤中栀子苷、黄芩苷、汉黄芩苷、黄芩素和汉黄芩素5种成分被完全分离；回归方程显示5种成分的峰面积与其浓度呈良好的线性；5种成分的加样回收率(n=15)分别为102.2%，97.56%，98.61%，97.85%，98.41%；RSD小于5.0%。结论：利用程序可变波长检测，建立了一种可靠的同时测定黄连解毒汤中5种标志性成分含量的HPLC方法。
关键词：栀子苷；黄芩苷；汉黄芩苷；黄芩素；汉黄芩素；黄连解毒汤；程序波长检测
中图分类号：R917&&& 文献标识码：A&&& 文章编号：08)02-0182-05
Simultaneous determination of geniposide and 4 flavonoids
in the traditional Chinese medicinal preparation Huanglian
Jiedu decoction by HPLC with programmed wavelength UV detection*
DENG Yuan-xiong1,2,LIU Li1,YU Sen1,XIE Lin1,LIU Xiao-dong1**
(1.Key Laboratory of Drug Metabolism and Pharmacokinetics,China Pharmaceutical University,Nanjing .The Medical College of Hunan Normal University,Changsha 410006,China)
Abstract Objective:To develop an HPLC method with programmed wavelength ultraviolet detection for the simultaneous determination of geniposide,baicalin,wogonoside,baicalein and wogonin in Huanglian Jiedu decoction,a traditional Chinese medicinal complex prescription which contains Rhizoma Coptidis,Radix Scutellariae,Cortex Phellodendri Chinensis and Fructus Gardeniae.Methods:The samples were separated on a Kromasil C18column(150 mm×4.6 mm,5 μm) by a linear gradient elution(0-8.5 min,86.5%B;8.5-17.0 min,86.5%B→80%B;17-30 min,80%B;30-40 min,80%B→60%B;40-51 min,60%B→52%B;51-55 min,52%B→42%B;55-60 min,42%B→86.5%B;60-65 min,86.5%B) using acetonitrile(A) and 5 mmol?L-1 &&&&&&&&&&&&&&&&&&&&&&&&&&&&&&&&&&&&&&&&&&&&&&&&&&&&&&&&&&&&&&&&&&&&&&&&&&&&&&&&&&&&&&&&&&&&&&&&&&&&&&&&&&&&&&&&&&&&&&&&&&&&&&&&&&&&&&&&&&&&&&&&&&&&&&&&&&&&&&&&&&&&&&&&&&&&&&&&&&&&&&&&&&&&&&&&&&&&&&&&&&&&&&&&&&&&&&&&&&&&&&&&&&&&&&&&&&&&&&&&&&&&&&&&&&&&&&&&&&&&&&&&&&&&&&&&&&&&&&&&&sodium dihydrogen phosphate [containing 0.05%(v/v)phosphoric acid](B) as mobile phase at a flow rate of 1.0 mL?min-1 and the eluate was detected by programmed wavelength(0-15 min,23815-50 min,276 nm).Results:The complete separation was obtained within 58 min for the five marker substances(geniposide,baicalin,wogonoside,baicalein and wogonin).Five regression equations showing linear relationships between peak-area and concentration of each marker were obtained.The average recoveries(n=15) of the markers listed above were 102.2%,97.56%,98.61%,97.85%,98.41%,respectively.The relative standard deviations were less than 5.0%.Conclusion:Very satisfactory and reproducible results are obtained for the simultaneous determination of the five markers in Huanglian Jiedu decoction.
Key words:geniposide;Huanglian Jprogrammed wavelength detection&&&&&&&&&&&&&&&&&&&&&&&&&&&&&&&&&&&&&&&&&&&&&&&&&&&&&&&&&&& &&&&&&&
香附药材质量相关性分析研究
江苏省高校自然基金重大基础研究资助项目(No.06KJA36022)；江苏省高校"青蓝工程"科技创新团队建设项目资助(2006年)
赵新慧，宿树兰，段金廒通讯作者Tel/Fax:(025);E-mail:dja@，刘陶世，侯鹏飞，尚尔鑫，唐于平
(南京中医药大学江苏省方剂研究重点实验室，南京 210046)
摘要目的：对收集的8个产地香附药材的质量进行分析与评价。方法：采用GC-MS法分析鉴定香附药材挥发性成分，分析条件为：DB-1701石英毛细管色谱柱（0.25 mm×30 m,0.25 μm），程序升温，进样口温度220 ℃，分流比100∶1，流速1 mL?min-1；采用HPLC法分析不同产地香附药材甲醇提取物的化学成分，分析条件为：Hedera ODS-2 C18色谱柱(4.6 mm×250 mm,5 μm)，甲醇(A)-水(B)系统为流动相，梯度洗脱[0~20 min，5%A~50%A；20~30 min，50%A~60%A；30~70 min，60%A~80%A；70~80 min，80%A~100%A]，流速1 mL?min-1，检测波长254 nm，柱温30 ℃。对8个不同产地香附药材的甲醇提取物化学成分特征进行相似度评价分析和聚类分析。结果：以GC-MS分析鉴定了香附挥发油中22个化合物；以HPLC法建立了不同产地香附甲醇提取物化学成分的特征图谱；相似度评价与聚类分析结果表明山东产香附与安徽、海南、浙江、江苏产香附距离较近，聚为一类，而河南与河北产香附与上述产地香附距离较远。结论：综合分析表明，地道产地山东香附与安徽、浙江和海南产香附在性状特征和化学成分信息方面均表现出较好的趋同性，与江苏、广西和河南产香附具有一定的趋同性，而河北安国香附在性状及聚类分析中均与山东香附距离最远，表现出明显的趋异性。本文研究结果为我国不同产地香附药材的检定、识别和质量评价提供了客观依据。
&关键词：香附；不同产地；GC-MS分析；HPLC分析
中图分类号：R917&&& 文献标识码：A&&& 文章编号：08)02-0187-06
Correlation studies on the quality of Rhizoma Cyperi*
ZHAO Xin-hui,SU Shu-lan,DUAN Jin-ao**,
LIU Tao-shi,HOU Peng-fei,SHANG Er-xin,TANG Yu-ping
(Jiangsu Key Laboratory for TCM Formulae Research,Nanjing University
of Traditional Chinese Medicine,Nanjing 210046,China)
Abstract Objective:To analyze the chemical components of Rhizoma Cyperi from different regions in China and to evaluate their qualities.Methods:GC-MS method was used to identify the components in essential oils of Rhizoma Cyperi from eight regions.The temperature programmed processes was performed on the column of DB-1701 quartz capillary column（0.25 mm×30 m,0.25 μm）.Split injection was conducted with a split ratio of 100∶1.The injector temperature was 220 ℃,flow rate of N2 was 1 mL?min-1.HPLC was used to analyze the components of methanol extract.And hierarchical cluster analysis was performed to find resemblance among Rhizoma Cyperi from different regions.The analytical method was developed on a Hedera ODS-2 C18 column(4.6 mm×250 mm,5 μm) and the mobile phase was consisted of CH3OH(A)& and H2O(B) using a linear gradient[0-20 min，5%A→50%A；20-30 min，50%A→60%A；30-70 min，60%A→80%A；70-80 min，80%A→100%A].The solvent flow rate was 1.0 mL?min-1 with UV absorbance detection 254 nm.The column temperature was set at 30 ℃.Results:Twenty-two principal constituents were identified in the volatile oils by GC-MS.RP-HPLC method was established for analysis of methanol extract of different resources Rhizoma Cyperi. Conclusion:Cluster analysis results showed that Rhizoma Cyperi from Anhui,Hainan,Zhejiang,Jiangsu,Guangxi could be gathered one group with Shandong sample based on the HPLC characteristic peaks.And samples from Henan and Hebei were most diversity with Shandong Rhizoma Cyperi.Conclusions:Rhizoma Cyperi from Anhui,Zhejiang and Hainan showed good convergence with the genuine area (Shandong)while Hebei sample showed obvious divergence with Shandong sample.The chemical information of genuine area (Shandong) sample showed some degree convergence with Rhizoma Cyperi from Jiangsu,Guangxi,and Henan.The results provided objective evidences for identifying and evaluating quality of Rhizoma Cyperi from different resources.
Key words:Rhizoma CGC-MSHPLC analysis
王琳蛇毒抗肿瘤蛋白心脏毒素的分离纯化与鉴定
吕萍，陈兴勇，赵宗阁，徐康森
第一作者Tel:(010);E-mail:luping123@
（中国药品生物制品检定所,北京100050）
摘要 目的：对蛇毒抗瘤蛋白的活性组分进行分离与鉴定。方法：采用RP-HPLC分离蛇毒抗瘤蛋白各组分，收集纯化组分Ⅱ。RP-HPLC及SDS-PAGE测定组分Ⅱ的纯度；MALDI-TOF质谱仪测定组分Ⅱ的相对分子质量；对组分Ⅱ进行N-末端氨基酸序列测定。结果：蛇毒抗瘤蛋白组分Ⅱ经RP-HPLC和SDS-PAGE分析为单一成分，MALDI-TOF 质谱仪测得其相对分子质量为6719.49，其N-末端氨基酸序列为L-K-C-N-K-L-V-P-L-F-Y-K-T-C-P。结论：经分离鉴定，蛇毒抗瘤蛋白组分Ⅱ为心脏毒素。
关键词：蛇毒抗瘤蛋白；RP-HPLC；氨基酸序列；心脏毒素
中图分类号：R917文献标识码：A文章编号：08)02-0193-03
Separation Purification and identification
of cardiotoxin in atranticance protein
La Ping,CHEN Xing-yong,ZHAO Zong-ge,XU Kang-sen
(National Institute for the Control of Pharmaceutical and
Biological Products,Beijing 100050,China)
Abstract Objective:Isolation,purification and identification of cardiotoxin in atranticance protein.Methods:Fractions of atranticance protein were isolated by RP-HPLC and the fraction Ⅱ was purified.Purity of the fraction Ⅱ was determined by RP-HPLC and SDS-PAGE.The relative molecular mass was determined by MALDI-TOF.N-teminal sequence of the fraction Ⅱ was analyzed.Results:The fraction Ⅱ was verified to be homogeneous by RP-HPLC and SDS-PAGE.The relative molecular mass of the fraction Ⅱ was 6719.49 by MALDI-TOF.The results of N-teminal sequence analysis were L-K-C-N-K-L-V-P-L-F-Y-K-T-C-P.Conclusion:The fraction Ⅱ in atranticance protein is cardiotoxin.
Key words:atranticanceRP-HPLC;cardiotoxin
HPLC法测定大鼠尿液中9-硝基喜树碱的浓度
陈军1,2，平其能2通讯作者Tel:（025）；E-mail: pingqn@，蔡宝昌1，刘敏玲2
（1.南京中医药大学药学院，南京 210029；2.中国药科大学药学院，南京 210009）
摘要 目的：建立HPLC法测定大鼠尿液中9-硝基喜树碱（9-NC）浓度。方法：尿液样品中加入内标喜树碱后，用甲醇-乙腈（1∶1）沉淀后离心取上清液进样。采用Diamonsil C18柱（250 mm×4.6 mm，5 μm）分离，流动相为乙腈-1%三乙胺（冰醋酸调pH至6.5）(45∶55)，流速1.0 mL?min-1，检测波长370 nm。测定静脉注射3 mg?kg-19-NC溶液和其脂质体溶液后大鼠尿液中原形药物的排泄情况。结果：线性范围72~18000 ng?mL-1，定量限为72 ng?mL-1。静脉注射9-NC溶液和脂质体溶液后24 h尿液中原形药物的累积排泄量分别为给药剂量的5.9%和7.6%。结论：本方法简便实用，定量准确，并成功应用于静脉注射9-NC脂质体后原形药物肾排泄的研究。
关键词：9-硝基喜树碱（9-NC）；脂质体；排泄；HPLC ；尿
中图分类号：R917&&& 文献标识码：A&&& 文章编号：08)02-0196-03
HPLC determination of the concentration of
9-nitrocamptothecin in rat urine
CHEN Jun1,2,PING Qi-neng2*,CAI Bao-chang1,LIU Min-ling2
(1.College of Pharmacy,Nanjing University of Chinese Medicine,Nanjing 210029,China;
2.College of Pharmacy,China Pharmaceutical University,Nanjing 210009,China)
Abstract Objective:To develop a novel HPLC method for the analysis of 9-nitrocamptothecin (9-NC) in rat urine.Methods:The urine samples were separated on a C18 column after being diluted by methanol-acetonitrile (1∶1).The mobile phase consisted of acetonitrile and 1% triethylamine (pH 6.5) (45∶55) at a flow rate of 1.0 mL?min-1.The UV detector was set at 370 nm.The ratios of cumulative excretion in urine to the administered dose were determined at different time following intravenous administration of 3 mg?kg-1 9-NC solution or liposome to rats.Results:The linear calibration curves were obtained in the concentration range of 72-18000 ng?mL-1.The limit of quantification was 72 ng?mL-1.After intravenous administration of 9-NC solution or liposome,the ratios of cumulative excretion in urine to the administered dose were 5.9% and 7.6%,respectively.Conclusion:The method which was simple,practical and accurate was successfully applied to the study of cumulative excretion of 9-NC into urine.
Key words:9-nitrocamptothecin(9-NC);HPLC;urine
反相高效液相色谱法测定人血浆中氟康唑的浓度及其应用
程晓华1，张红2，胡晓2，徐文炜2，熊玉卿2
通讯作者Tel:(;E-mail:.cn
（1.南昌大学第一附属医院科教科，南昌 .南昌大学医学院临床药理研究所，南昌 330006）
摘要目的：建立氟康唑人血浆中药物浓度的高效液相色谱测定方法,并用于氟康唑人体药代动力学研究。方法：使用固相萃取高效液相色谱紫外检测法，样品经Bond elut固相萃取小柱处理。色谱柱为Diamonsil C18柱（4.6 mm×150 mm，5 μm）,流动相：0.01 mol?L-1磷酸二氢钾（1000 mL 0.01 mol?L-1磷酸二氢钾加入200 μL三乙胺）-乙腈-甲醇（60∶24∶16），流速为1.0 mL?min-1,柱温为30 ℃，紫外检测波长267 nm，内标为非那西丁。结果：氟康唑血浆浓度测定方法的线性范围为0.1~9.6 μg?mL-1,线性关系良好（r=0.9997），最低检测浓度为0.1 μg?mL-1（以S/N&4计），方法回收率为93.7%~102.1%，日内和日间差异均小于6%。结论：本文采用的高效液相色谱紫外检测法灵敏度高、重复性好，能快速可靠地测定氟康唑血药浓度，适用于氟康唑的血药浓度监测和人体药代动力学研究。
关键词：氟康唑；血药浓度；高效液相色谱
中图分类号：R917&&& 文献标识码：A&&& 文章编号：08)02-0199-03
RP-HPLC determination of fluconazole concentrations
in human plasma and its application
CHENG Xiao-hua1,ZHANG Hong2,HU Xiao2,XU Wen-wei2,XIONG Yu-qing2*
(1.Department of Science and Education,The First Affiliated Hospital of Nanchang University,Nanchang 330006,China;
2.Institute of Clinical Pharmacology,Medical College of Nanchang University,Nanchang 330006,China)
Abstract Objectives:To establish a method for the determination conacentration of fluconazole in human plasma by HPLC and apply it to the pharmacokinetic study of fluconazole.Methods:Fluconazole in plasma was extracted with Bond elut solid phase extraction,HPLC instrument was adopted with C18 reversed-phase column (4.6 mm×150 mm，5 μm) and monitored by UV.The mobile phase composed of 0.01 mol?L-1 KH2PO4 (1000 mL 0.01 mol?L-1KH2PO4 with 200 μL triethylamine)-acetonitrile-methanol (60∶24∶16),eluated with a flow rate of 1.0 mL?min-1,detection wavelength was 267 nm with phenacetin as internal standard.Results:The calibration curve of fluconazole was in the range of 0.1-9.6 μg?mL-1 (r=0.9997).The detection limit was 0.1 μg?mL-1(S/N &4).The recoveries of methodology were 93.7%-102.1% with intra-day RSD and inter-day RSD were less than 6%.Conclusions:The method has good sensitivity,precision and simple.It is shown to be suitable for pharmacokinetic studies of fluconazole in human and the clinical monitoring of the plasma concentration of fluconazole.
Key words:fluconazole;plasma cHPLC
液相色谱-质谱/质谱联用法测定健康志愿者血清中阿德福韦
王海生1，高彦慧2，孙德清1，王本杰3，郭瑞臣3
通讯作者Tel:(6;Fax:(5;E-mail:
（1.山东大学第二医院药剂科，济南 250033；2.山东大学药学院，济南 250012；
3.山东大学齐鲁医院临床药理研究所，济南 250012）
摘要 目的：建立测定人血清中阿德福韦的液相色谱-质谱/质谱联用(LC-MS/MS)方法。方法：血清样品经甲醇沉淀蛋白，上清液吹干，200 μL流动相复溶，离心，取40 μL进样。色谱柱为Diamonsil C18 柱（250 mm×4.6 mm，5 μm），流动相为甲醇-水-甲酸（20∶80∶0.1,v/v/v），流速0.6 mL?min -1，采用电喷雾离子化四极杆串联质谱，多反应监测方式测定样品浓度。监测离子对分别为m/z 274→m/z 162（阿德福韦）和m/z 226→m/z 135 （内标阿昔洛韦）。结果：阿德福韦在1.25~160 μg?L-1浓度范围内线性关系良好（r=0.9992，n=5），最低定量限为1.25 μg?L-1。低、中、高3种浓度质控样品的日内、日间精密度小于8.64%，方法回收率99.20%~101.98%，阿德福韦提取回收率56.50%~59.26%。结论：该方法灵敏度高，定量准确，适用于阿德福韦酯人体药代动力学研究。
关键词：阿德福韦；液相色谱-质谱/质谱联用；血清药物浓度
中图分类号：R917&&& 文献标识码：A&&& 文章编号：08)02-0202-05
Determination of adefovir in human serum by
liquid chromatography-tandem mass spectrometry
WNAG Hai-sheng1,GAO Yan-hui2,SUN De-qing1,WANG Ben-jie3,GUO Rui-chen3*
(1.Department of Pharmacy,the Second Hospital of Shandong University,Jinan .Pharmaceutics College of Shandong University,Jinan .Institute of Clinical Pharmacology,
Qilu Hospital of Shandong University,Jinan 250012,China)
Abstract Objective:To develop a liquid chromatography-tandem mass spectrometry (LC-MS/MS) method for the determination of adefovir in human serum.Methods:The analyte was isolated from serum by protein precipitation with methanol,the supernatant was evaporated to dryness and reconstituted with 200 μL of mobile phase,then 40 μL was injected for analysis.A Diamonsil C18 column（250 mm×4.6 mm，5 μm）and mobile phase consisted of methanol-water-formic acid (20∶80∶0.1,v/v/v) at a flow rate of 0.6 mL?min-1 were used to separate adefovir and IS.Electrospray ionization (ESI) source was applied and operated in the positive ion mode.Multiple reaction monitoring (MRM) mode with the transition of m/z 274→m/z 162 and m/z 226→m/z 135 were used to quantify adefovir and aciclovir (IS),respectively.Results:A good linearity was obtained in the concentration range of 1.25-160 μg?L-1（r=0.9992,n=5）.The lower quantitative limit was 1.25 μg?L-1.The inter-and intra-day RSDs were less than 8.64%,the method recoveries were within 99.20%-101.98% and the extraction recoveries were within 56.50%-59.26%.Conclusion:The method is sensitive and acuurate,and proves to be suitable for human pharmacokinetics study of adefovir dipivoxil.
Key words:adefovir;LC-MS/MS;serum concentration
LC-MS/MS法测定犬血浆中左卡尼汀
王大为，武洁，黄厚才，王志刚，胡春萍
第一作者Tel：(025)；E-mail:
（江苏省中医药研究院药物代谢与临床药学研究室，南京 210028）
摘要 目的：建立Beagle犬血浆中左卡尼汀浓度的LC-MS/MS测定方法。方法：待测血浆50 μL经甲醇沉淀除去蛋白，离心，取上清液10 μL进样分析。流动相为甲醇-0.05%醋酸溶液（30∶70），色谱柱为江苏汉邦氰基柱（150 mm×4.6 mm，5 μm），流速为1.0 mL?min-1，LC-MS/MS多反应离子检测，正离子模式，用于定量分析的离子分别是左卡尼汀m/z 162.2 → 84.7[M+H]和茶碱m/z 181.2 →124.0[M+H]。结果：血浆中杂质不干扰样品和内标的测定，样品分析时间小于5 min，左卡尼汀的线性范围为0.5~200 μg?mL-1，方法的回收率大于80%，批内和批间的RSD均小于10%，稳定性符合生物样品测定要求。结论：该方法经考察符合血浆样品的测定要求，可以应用于血药浓度的测定和药代动力学研究
关键词：左卡尼汀；LC-MS/MS法；血药浓度
中图分类号：R917&&& 文献标识码：A&&& 文章编号：08)02-0207-04
LC-MS/MS determination of L-carnitine in dog plasma
WANG Da-wei,WU Jie,HUANG Hou-cai,WANG Zhi-gang,HU Chun-ping
(Lab of Pharmacokinetics and Clinical Pharmacy,Jiangsu Provincial Institute of
Traditional Chinese Medicine,Nanjing 210028,China)
Abstract Objective:To develop a sensitive and specific LC-MS/MS method for determination of L-carnitine in Beagle dog.Methods:The analyte was treated by methanol precipitation to remove protein component from dog plasma,then separated on a cyano-column.The mobile phase consisted of methanol-0.05% acetic acid solution (30∶70),at a flow rate of 1.0 mL?min-1.A mass spectrometer equipped with electrospray ionization source was used as detector and operated in the positive ion mode.In multiple reaction monitoring (MRM) mode,the ion combinations of m/z 162.2 → 84.7 and m/z 181.2 →124.0 was used to qualify L-carnitine and internal standard (theophylline),respectively.Results:Chromatograms showed no endogenous interfering peaks with the respective blank dog plasma samples.Each analysis was completed within 5 min.The calibration was linear in the concentration range within 0.5-200 μg?mL-1.The intra-batch and inter-batch RSD were less than 10%.The recovery of the extraction was more than 80%.Conclusions:The method is proved to be suitable for pharmacokinetics of L-carnitine with specificity,quickness,and higher sensitivity over the previously reported methods.
Key words:L-carnitine；LC-MS/MS；plasma concentration
HPLC-MS/ESI法测定人血浆中文拉法新及其代谢产物氧
去甲基文拉法新对映体血药浓度
刘文1,2，王峰1，李焕德1
通讯作者Tel：(；Fax：（0731）4436720；E-mail:.cn
(1.中南大学湘雅二医院临床药学教研室，长沙 .湖南省人民医院药剂科，长沙 410005 )
摘要 目的：建立反相高效液相色谱-质谱法同时测定人血浆中文拉法新(VEN)及其主要代谢产物氧去甲基文拉法新(ODV)对映体的浓度。方法：使用万古霉素手性柱（CHRIOBIOTIC V TM）(250 mm×4.6 mm,5 μm)，以甲醇-醋酸铵缓冲液(30 mmol?L-1) (15∶85，pH 6.0)为流动相对两化合物进行手性拆分，流速设为1.0 mL?min-1，柱后分流比为3∶1。采用质谱电喷雾电离正源（ESI+）将样品离子化，选择性离子监测（SIM）准分子离子峰。结果：在所建立的色谱条件下，VEN与ODV得到很好的手性分离。S-(+)与R-(-)-VEN在5.0~400 ng?mL-1，S-(+)与R-(-)-ODV在4.0~300 ng?mL-1 范围内线性关系良好，相关系数均大于0.9991； 萃取回收率均大于76%；方法回收率均大于92%；最低检测浓度：S-(+)与R-(-)-VEN 为1.0 ng?mL-1，S-(+)与 R-(-)-ODV 1.5 ng?mL-1；日内及日间RSD均小于9%。结论：本方法简单、快速、灵敏、准确，可用于VEN人体内立体选择性代谢的研究。
关键词：文拉法新（VEN）；氧去甲基文拉法新(ODV)；手性拆分；万古霉素手性柱；HPLC-MS/ESI
中图分类号：R917&& &文献标识码：A&&& 文章编号：08)02-0211-05HPLC-MS/ESI simultaneous determination of venlafaxine and its metabolite O-desmethylvenlafaxine
enantiomers in human plasma
LIU Wen1,2,WANG Feng1,LI Huan-de1*
(1.Clinical Pharmaceutical Research Institute,Second Xiangya Hospital,Central South University,Changsha .Department of Pharmacy,Hunan Provincal Peoples Hospital,Changsha 410005,China)
Abstract Objective:To establish an HPLC-MS/ESI method for simultaneous stereoselective analysis of venlafaxine(VEN) and its major metabolite O-desmethylvenlafaxine(ODV) enantiomers in human plasma.Method:The CHRIOBIOTIC VTM (250 mm×4.6 mm,5 μm) column was used with mobile phase constituted of 30 mmol?L-1 ammonium acetate-methanol (85∶15,pH 6.0) with a flow rate of 1.0 mL?min-1 and the postcolumn splitting ratio was 3∶1.The compounds were ionized in the electrospray ionization (ESI) ion source of the mass spectrometer and detected in the selected ion recording (SIR) mode.Result:The enantiomers of VEN and ODV were completely separated under the present method.Calibration curves in spiked plasma were linear from 5.0-400 ng?mL-1 for S-(+)-VEN and R-(-)-VEN,4.0-300 ng?mL-1 for S-(+)-ODV and R-(-)-ODV,respectively.All of them with coefficients of determination above 0.9991.The average extraction recoveries for all the four analytes were above 76%.The methodology recoveries were higher than 92%.The limit of detection were 1.0 ng?mL-1 for S-(+)-VEN and R-(-)-VEN,1.5 ng?mL-1for S-(+)-ODV and R-(-)-ODV,respectively.The intra-day and inter-day relative standard deviations were less than 9%.Conclusion:The method is accurate,sensitive and reliable for the stereoselective metabolism study of the VEN in human plasma.
Key words:venlafaxine(VEN);O-desmethylvenlafaxine(ODV);vancHPLC-MS/ESI
反相高效液相色谱法测定大鼠血浆及子宫组织中达那唑的药物浓度
浙江省科技厅重点项目资助（204C30039）
叶轶青，林俊，张信美，杨峰亮，虞和永
通讯作者Tel:(1;E-mail:yuhy@(浙江大学医学院附属妇产科医院，杭州 310006)
摘要 目的：建立反相高效液相色谱法测定大鼠血浆及子宫组织样品中达那唑药物浓度。方法：生物样本经沉淀蛋白后，上清液直接进样。色谱条件：甲醇-水(78∶22) 为流动相，用Agilent Zorbax Eclipse XDB-C18(250 mm×4.6 mm，5 μm)色谱柱进行分离，284 nm检测，流速1.0 mL?min-1。结果：血浆中达那唑的线性范围为31.25~2500 ng?mL-1，定量限为31.25 ng?mL-1；子宫组织中达那唑的线性范围为62.5~2500 ng?g-1，定量限为62.5 ng?g-1；方法回收率均大于90%。结论：本方法简单、准确，专属性强，灵敏度高，可用于临床药代动力学研究。
关键词：达那唑；高效液相色谱法；血浆；子宫组织
中图分类号：R917&&& 文献标识码：A&&& 文章编号：08)02-0216-03
HPLC determination of danazol in rat plasma and uterus tissue*
YE Yi-qing，LIN Jun,ZHANG Xin-mei,YANG Feng-liang,YU He-yong**
(Women Hospital,Medicine School,Zhejiang University，Hangzhou 310006,China)
AbstractObjective:To develop a method for determination of danazol in rat plasma and uterus tissue.Methods:Plasma and uterus tissue samples were prepared by precipitating protein in plasma and uterus.The method was performed on an Agilent Zorbax Eclipse XDB-C18(250 mm×4.6 mm，5 μm).The mobile phase consisted of methanol-water (78∶22).The detector was set at 284 nm and the flow rate was 1.0 mL?min-1.Results:The linear calibratiiv curves were observed in the concentration range of 31.25-2500 ng?mL-1 in plasma and 62.5-2500 ng?g-1 in uterus tissue,respectively.The lower limits of quantification were 31.25 ng?mL-1 and 62.5 ng?g-1,respectively.The relative recoveries were more than 90%.Conclusion:The method is accurate and convenient.It can be used to determine danazol for studying their preclinical pharmacokinetics.
Key words:HPLC;uterus tissue
流动注射-化学发光法测定片剂、人血清
及尿液中6-巯基嘌呤的含量
教育部博士点学科基金项目 (No.)
第一作者Tel: (;E-mail:
孙汉文1，苏明1，李丽清1,2，陈雪艳1
（1.河北大学化学与环境科学学院河北省分析科学技术重点实验室，保定 071002； 2.泰山学院化学系，泰安 271021）
摘要目的：研究6-巯基嘌呤-高锰酸钾-甲醛-多聚磷酸体系的化学发光行为与机理，建立流动注射-化学发光法测定片剂、人血清与尿液中6-巯基嘌呤的含量。方法：采用6-巯基嘌呤-高锰酸钾-甲醛-多聚磷酸化学发光体系，基于化学发光强度与浓度间的线性关系对6-巯基嘌呤加以定量测定。结果：校准曲线的线性范围为1.0×10-8~1.0×10-5 g?mL-1，检出限为6×10-9 g?mL-1；对2.0×10-7 g?mL-1 6-巯基嘌呤进行11次平行测定，RSD为1.7%；片剂、人血清和尿液加样回收率在95.0%~111.3%范围内，RSD为1.8%~2.2%。结论：本方法简便、灵敏、可靠，可用于6-巯基嘌呤的常规检测及药代动力学研究。
关键词：流动注射；化学发光；6-巯基嘌呤；药剂；血清；尿液
中图分类号：R917&&& 文献标识码：A&&& 文章编号：08)02-0219-04
A flow injection chemiluminescence method for determination
of 6-mercaptopurine in its tablets,human serum and urine*
SUN Han-wen1,SU Ming1,LI Li-qing1,2,CHEN Xue-yan1
(1.College of Chemistry and Environmental Sciences,Hebei University,Key Laboratory of Analytical Science and Technology of Hebei Province,Baoding .Department of Chemistry,Taishan University,Tai an 271021,China)
Abstract Objective：To study chemiluminescence characteristic and mechanism of the potassium permanganate-formaldehyde-6-mercaptopurine polyphosphate system and to establish a novel method for determination of 6-mercaptopurine in pharmaceutical preparations,human serum and urine by flow injection chemiluminescence techniqure.Methods:Potassium permanganate-formaldehyde 6-mercaptopurine polyphosphate was adopted in chemiluminescence system.6-mercaptopurine was quantitatived based on linear relationship between the chemiluminescence intensity and the concentration.Results:The linear range of the calibration curve was 1.0 ×10-8-1.0×10-5 g?mL-1,and the detection limit was 6×10-9 g?mL-1.The RSD was 1.7% for 11 measurements at 2.0×10-7 g?mL-1 6-mercaptopurine standard solution.The recoveries for spiked pharmaceutical preparations,serum and urine were in the range of 95.0%-111.3%.The results agree well with those obtained by the Pharmacopoeia standard method.Conclusion:The proposed method is simple,sensitive and reliable.It can be applied for routine determination of 6-mercaptopurine and pharmacokinetic study.
Key words:flow-6-pharmacurine
转基因山羊羊乳中重组人乳铁蛋白性质的检定与研究
李佐刚，汤瑶，孙旭，闻镍，于敏，史兴昌，李响，王秀文，王军志，李波
第一作者Tel:(010)2;Fax:(010);E-mail:
（中国药品生物制品检定所国家药物安全评价监测中心，北京100176）
摘要 目的：检定与研究转基因山羊CLF123-1羊乳中重组人乳铁蛋白（rhLF）及其分子特性。方法：利用SDS-PAGE，Western-blotting及Edman降解法测定分析转基因山羊羊乳中rhLF的相对分子质量、免疫学特性和N-末端15个氨基酸残基；利用紫外分光光度法比较rhLF、天然人乳铁蛋白(hLF)与Fe3+离子结合的动力学过程，测定Fe3+与LF发生结合反应达到平衡状态后在279 nm和465 nm的吸收度值，Fe3+与LF的物质的量比值分别为：0∶1，0.5∶1，1∶1，2∶1，4∶1。结果：rhLF的相对分子质量为(8.06±0.15)万（2次实验，6条电泳谱带计算结果）；Western-blotting结果显示rhLF可特异地与兔抗人LF抗体发生特异性结合；rhLF的N-末端1~15个氨基酸残基的序列为G R R R R S V Q W X T V S Q P；rhLF和hLF与Fe3+结合特性与趋势几乎完全一致。结论：本文所研究的转基因山羊羊乳中的乳铁蛋白是与人乳铁蛋白分子特性一致的rhLF。
关键词：重组人乳铁蛋白（rhLF）；转基因山羊； SDS-PAGE；免疫印迹法；N-末端测序；生物反应器；铁结合蛋白
中图分类号：R917&& &文献标识码：A&&& 文章编号：08)02-0223-04
Identification and characterization of recombinant
human lactoferrin in the milk of transgenic goats
LI Zuo-gang,TANG Yao,SUN Xu,WEN Nie,YU Min,SHI Xing-chang,LI Xiang,
WANG Xiu-wen,WANG Jun-zhi,LI Bo
（National Center for Safety Evaluation of Drug,National Institute for the Control of
Pharmaceutical and Biological Products，Beijing 100176,China）
Abstract Objective:To identify and characterize the recombinant human lactoferrin (rhLF) in the milk of transgenic goats.Methods:rhLF was characterized and analyzed by SDS-PAGE,Western-blotting and N-terminal sequencing with Edman degradation.The iron-binding properties of natural human lactoferrin (hLF) and rhLF at the mole ratio 0∶1,0.5∶1,1∶1,2∶1 and 4∶1 (Fe3+:LF) were compared by using UV absorbance at 279 nm and 465 nm.Result: ：The relative molecular mass of rhLF was (8.06±0.15)×104 (two tests and n=6).The Western-blotting showed that rhLF can specially bind with rabbit anti hLF antibody.N-terminal sequence amino acid residues from 1-15 were G R R R R S V Q W X T V S Q P.The iron-binding of rhLF and hLF was highly similar.Conclusion:The protein with relative molecular mass& (8.06±0.15)×104 in the milk of transgenic goalt is rhLF.
Key words:recombinant human lactoferrin(rhLF);SDS-PAGE;Western-BN-terminal sequence；iron-binding
吡虫啉在枸杞中的残留动态研究
国家科技部社会公益研究专项（2004DIB1J039）；国家中医药管理局项目（02-03ZP03）
陈美艳，于晶，徐荣，周峰，薛健，陈建民
陈君，通讯作者Tel：(010)；E-mail：
（中国医学科学院中国协和医科大学 药用植物研究所，北京 100094）
摘要 目的：研究20%吡虫啉可溶性液剂在枸杞中的消解动态。方法：采用高效液相色谱法，样品经甲醇提取，二氯甲烷萃取，层析柱净化，采用十八烷基键合硅胶柱（4.6 mm×250 mm，5 μm），流动相为0.1%磷酸-乙腈，梯度洗脱；检测波长270 nm。结果：样品的添加回收率为87.6%~96.0%，RSD为1.5%~3.1%。吡虫啉在枸杞中的半衰期为1.63 d，施药10 d后残留量降至0.0126 mg?kg-1，最终残留量在0.002 mg?kg-1以下。结论：在正常喷药浓度的加倍剂量2000倍条件下，安全采收间隔期为5 d以上。
关键词：高效液相色谱法；吡虫啉；枸杞；残留
中图分类号：R917&&& 文献标识码：A &&&文章编号：08)02-227-04
Study on residue trends of imidacloprid in Lycium barbarum L.*
CHEN Mei-yan,YU Jing,CHEN Jun**,XU Rong,ZHOU Feng,XUE Jian,CHEN Jian-min
(Institute of Medicinal Plant Development,Peking Union Medicinal College,Beijing 100094,China)
Abstract Objective:To study residue trends of 20% imidacloprid SL in Lycium barbarum L. Method:It was carried out by HPLC.Imidacloprid was extracted with methanol,dichloromethane,cleaned up with chromatography column,then separated on Spherisorb C18（4.6 mm×250 mm,5 μm）column by using 0.1% phosphoric acid-acetonitrile with a gradient elution,detected at 270 nm.Results:The fortified average recoveries varied from 87.6%-96.0%,and RSD was 1.5%-3.1%.The half-life of imidacloprid in Lycium barbarum L. was 1.63 d,the residue amount of imidacloprid was 0.0126 mg?kg-1 after 10 d,the final residue amount was less than 0.002 mg?kg-1.Conclusion:When doubled normal dilution of 2000 is applied,the safe interval period is more than 5 d.
Key words：HPLC;imidacloprid;Lycium barbarum L.;residue
紫杉醇脂质体药物含量及包封率的测定
杨涛1,2，金大德2，崔福德1通讯作者Tel:(024);E-mail:
（1.沈阳药科大学药剂教研室，沈阳，110016；2.首尔国立大学药学院，首尔，韩国，151-742）
摘要目的：建立紫杉醇脂质体含量及包封率的测定方法。方法：采用RP-HPLC法，LiChrospher 100反相C18 （250 mm×4.6 mm,5 μm）色谱柱，乙腈-水（50∶50）为流动相，流速为1.0 mL?min-1，紫外检测波长为227 nm，柱温为室温。利用混合有机溶剂对紫杉醇脂质体进行破坏，直接用HPLC法确定紫杉醇的含量。采用低速和超速离心法相结合的方法分离游离药物，确定脂质体中紫杉醇的包封率。结果：在脂质体平均粒径不到200 nm的条件下，通过离心法可以将游离紫杉醇与脂质体完全分离。紫杉醇与辅料及溶剂峰分离良好，线性范围为0.04~1.0 μg?mL-1；研究了负电荷对紫杉醇脂质体的作用，发现1%的磷脂酰丝氨酸(PS)能够提高紫杉醇的含量到(23.6±1.0) μg?mg-1，提高紫杉醇脂质体的包封率到(86.0±1.8)%。结论：所用方法简便、准确，可用于紫杉醇脂质体的含量及包封率测定。
关键词：紫杉醇；脂质体；包封率
中图分类号：R917&&& 文献标识码：A&&& 文章编号：08)02-0231-04
Determination of content and entrapment
efficiency of paclitaxel loaded liposome
YANG Tao1,2,KIM Dae-duk2,CUI Fu-de 1*
(1.College of Pharmacy,Shenyang Pharmaceutical University,Shenyang 110016,China;2.College of Pharmacy,
(2.Seoul National University,Seoul,South Korea,151-742)
Abstract Objective:To develop a method for the determination of content and entrapment efficiency of paclitaxel loaded liposome.Methods:The separation of free paclitaxel from liposome was performed with a method combining low-speed centrifugation and ultracentrifugation method to determine the entrapment efficiency of paclitaxel-loaded liposome.After the liposome was destroyed by mixed organic solvent, the paclitaxel content in liposome was detected by RP-HPLC method at 227 nm and the flow rate of mobile phase was 1.0 mL?min-1. LiChrospher 100 RP-18 column（250 mm×4.6 mm,5 μm）was used as analytical column and the mobile phase was composed of acetonitrile and water (50∶50),at room temperature.Results:The paclitaxel can be well separated from the liposome when the mean particle size of liposome was less than 200 nm.The effect of negative charge on the paclitaxel-loaded liposome was studied,which showed that 1% phosphatidylserine (PS) can increase the paclitaxel content in freeze-dried liposome powder to (23.6±1.0) μg?mg-1 and the entrapment efficiency of paclitaxel to (86.0±1.8)%,respectively.Conclusion:The method is accurate and can be used to determine the content and entrapment efficiency of paclitaxel loaded liposome.
Key words:paclitaxel;entrapment efficiency
流动注射纳米微反应器化学发光法测定盐酸曲马多
重庆市教委资助项目（No.KJ061306）；重庆市科技攻关计划项目；发光与
实时分析重庆市重点实验室开放基金项目；长江师范学院资助项目
第一作者Tel：（023）；E-mail：
石文兵，杨季冬，江虹，徐建华
（长江师范学院化学系，涪陵 408003）
摘要目的：建立盐酸曲马多的化学发光测定新方法。方法：在酸性条件下，盐酸曲马多分子中氮原子被质子化后与阴离子AuCl-1形成离子缔合物，该缔合物被二氯甲烷带入鲁米诺的氯化十六烷基三甲基铵反胶束纳米微反应器中，离解出来的AuCl-1立即与鲁米诺产生化学发光。在一定浓度范围内，发光强度与盐酸曲马多的含量呈线性关系，从而间接测定盐酸曲马多的含量。结果：在优化的试验条件下，线性范围为 0.001~30 μg?mL-1，检出限（3σ）为 0.02 ng?mL-1，对浓度为1.0 μg?mL-1 的盐酸曲马多进行11次平行测定，RSD为1.3%。结论：该法已成功用于片剂、注射液和生物体液中盐酸曲马多的测定。
关键词：纳米微反应器；盐酸曲马多；化学发光
中图分类号：R917&&& 文献标识码：A&& &文章编号：08)02-0235-04
Flow-injection chemiluminescence with nanometer microreactor
analysis of tramadol hydrochloride*
SHI Wen-bing,YANG Ji-dong,JIANG Hong,XU Jian-hua
（Department of Chemistry,Yangtze Teachers College,Fuling 408003,China）
Abstract Objective:To establish a flow injection chemiluminescence (CL) method for the determination of tramadol hydrochloride.Methods：In acidic condition,the nitrogen in tramadol hydrochloride was easily protonated forming ion-complex with negative ion AuCl-4,the ion-complex was extacted and carried by dichloromethane,when the ion-complex entered a reversed micellar nanometer microreactor of cetyltrimethylammonium chloride containing luminol,the dissociated AuCl-4 reacted with luminol and produced analytical chemiluminescence.Results：In the optimum conditions,the linear range was 0.001 to 30 μg?mL-1 and the limit of detection was 0.02 ng?mL-1 with a relative standard deviation (n=11) of 1.3% for 1.0 μg?mL-1 tramadol hydrochloride.Conclusion：The method has been applied to the determination of the studied drug in tablets,injections and biological fliuds successfully.
Key words:nanometertrchemiluminescence
国家自然科学基金资助项目()
王传琴，张现，王桃玲
吴守国通讯作者Tel:(;E-mail:sgwu@
(中国科学技术大学化学系，合肥 230026)
摘要目的：研究肾上腺素(EP)在β-环糊精修饰聚乙酰苯胺玻碳电极(β-CD/PNAANI/GCE)上的电化学行为，建立一种新的测定EP的电化学分析方法。方法：用循环伏安法研究EP在修饰电极上的氧化还原特性，用差分脉冲伏安法直接测定肾上腺素的含量。结果：该修饰电极能很好地催化EP，与裸玻碳电极(GCE)相比，还原峰电流增强近30倍。在pH 7.5磷酸盐缓冲液中，还原峰电流与EP的浓度在6.0×10-6~1.0×10-4 mol?L-1范围内呈良好的线性关系，其线性回归方程为Ip=1.68+6.92×10-6CEP ,相关系数为0.9975，检测限为1.0×10-7 mol?L-1。回收率在97.5%~104.5%之间。结论：该方法操作简单，可用于注射液中盐酸肾上腺素含量的测定，结果令人满意。
关键词：β-环糊精修饰电极；肾上腺素（EP）；伏安法
中图分类号：R917&&& 文献标识码：A&&& 文章编号：08)02-0239-04
Direct determination of epinephrine content in injection
with β-cyclodextrin modified electrode*
WANG Chuan-qin,WU Shou-guo**,ZHANG Xian,WANG Tao-ling
(Department of Chemistry,University of Science and Technology of China,Heifei 230026,China)
Abstract Objective:To investigate the electrochemical behaviors of epinephrine (EP) at the β-cyclodextrin modified poly(N-acetylaniline) (PNAANI) glassy carbon electrode (GCE) (β-CD/PNAANI/GCE) and establish a novel electroanalytical technique for the determination of EP.Methods:The redox characteristics of epinephrine (EP) at the modified electrode were investigated by cyclic voltammetry (CV).Epinephrine content was determined by differential pulse voltammetry (DPV).Results:The β-cyclodextrin modified electrodes showed an excellent electrocatalytic activity for the reduction of epinephrine (EP).The reduction peak height of EP was almost increased by 30 times compared with the bare glassy carbon electrode.In pH 7.5 phosphate buffer solution (PBS),the cathodic current increased linearly with the concentration of EP in the range of 6.0×10-6-1.0×10-4 mol?L-1.The linear regression equation was Ip=1.68+6.92×10-6 CEP ,with correlation coefficient of 0.9975.The detection limit was 1.0×10-7 mol?L-1with a good recovery between 97.5% and 104.5%.Conclusion:The proposed method is simple,sensitive and reproducible and is applied to measure the content of epinephrine in injection.
Key words:β-cyclodextriepinephrine(EP);voltammetry
高效毛细管电泳法测定磺胺类药物的离解常数及其制剂的含量
泰山医学院博士启动基金（）
第一作者Tel:(-8004;E-mail:
李玉琴1，张传港1，宗素艳3，崔英杰2，贾宝秀1，赵晓明2，曹明亮1，齐永秀1
(1.泰山医学院药学院，泰安271016；2.泰山医学院生命科学研究所，泰安 .
(2.南京工业大学制药与生命科学学院，南京 210009)
摘要 目的：采用毛细管电泳法测定磺胺甲唑(SMZ)、磺胺嘧啶(SD)和甲氧苄啶(TMP)的离解常数及其在制剂中的含量。方法：采用未涂层的弹性石英毛细管柱（60.2 cm×75 μm,有效长度50 cm），柱温25 ℃，正极压力进样，检测波长214 nm。将3种化合物的有效电泳淌度与pH进行非线性拟合，测定其离解常数；最佳的分离条件为：50 mmol?L-1磷酸二氢钠（pH 6.0）缓冲液，分离电压27.5 kV，在此条件下测定其在制剂中的含量。结果：SMZ、SD、TMP的离解常数分别为5.69，6.36，6.68；在0.1~1000 μg?mL-1的浓度范围内线性关系良好（相关系数：0.9992~0.9999），回收率为95.6%~105.0%。结论：该方法简便、快速、准确,可用于测定3种磺胺类药物的解离常数及其在制剂中的含量。
关键词：高效毛细管电泳；磺胺甲唑（SMZ）；磺胺嘧啶（SD）；甲氧苄啶（TMP）；pKa
中图分类号：R917&&& 文献标识码：A&&& 文章编号：08)02-0243-04
HPCE determination of dissociation constants
of sulfonamides and their contents*
LI Yu-qin1，ZHANG Chuan-gang1，ZONG Su-yan3，CUI Ying-jie2，
ZHAO Xiao-ming2，CAO Ming-liang1，QI Yong-xiu1
(1.Pharmacy College,Taishan Medicine College,Taian .Bioscience Institute of Taishan Medicine College,Taian 271016,C3.College of Life Science and Pharmaceutical Engineering
,Nanjing University of Technology,Nanjing 210009,China)
Abstract Objective:To develop a simultaneous determination the dissociation constant values of sulfamethoxazole(SMZ),sulfadiazine(SD) and trimethoprim(TMP),and the contents in their preparations by HPCE.Method:A fused silica capillary column (60.2 cm×75 μm,effective length 50 cm) was used,the cartridge temperature was 25 ℃,sample was introduced from the anode with pressure injection,the UV detection wavelength was 214 nm.The dependence of effective mobility of the three compound on pH was investigated,and their apparent dissociation constant values determined by the best separation was achieved with a running buffer of 50 mmol?L-1 NaH2PO4 (pH 6.0) and at the applied voltage of 27.5 kV for determination the contents of the three compounds.Result:The dissociation constant values(pKa) of SMZ,SD and TMP were 5.69,6.36 and 6.68,respectively.The linear concentration range of the three compounds was 0.1-1000 μg? mL-1 with a correlation coefficient of 0.9992~0.9999.The recoveries of the three analytes were 95.6%-105.0%.Conclusion:The proposed method is simple,fast and accurate for determination the dissociation constant values of sulfonamides and their contents.
Key words:HPCE;sulfamethoxazole(SMZ);sulfadiazine(SD);trimethoprim(TMP);pKa
聚伊文思蓝膜修饰玻碳电极在抗坏血酸共存时测定去甲肾上腺素
国家自然科学基金资助项目（）；福建省卫生厅青年基金资助项目（2006111）
林丽清，姚宏，庄茜，李巍，林新华
通讯作者Tel：(6；E-mail:
（福建医科大学药学院药物分析系，福州350004）
摘要目的：研究聚伊文思蓝(Evans Blue) 膜修饰玻碳电极对去甲肾上腺素（NE）和抗坏血酸（AA）的电化学行为，建立测定NE含量的电化学分析新方法。方法：采用循环伏安法研究NE和AA在聚伊文思蓝膜修饰电极上的电化学行为，以差示脉冲伏安对NE的含量进行测定。结果：聚伊文思蓝膜修饰电极对NE 和AA有显著的增敏和电分离作用，氧化峰电位差为282 mV。在pH 5.0的磷酸盐缓冲液中，氧化峰电流与NE浓度在5.0×10-7~1.8×10-5 mol?L-1范围内呈良好的线性关系，检测限为4.0×10-8 mol?L-1。结论：该修饰电极在抗坏血酸共存时可测定NE，有效消除其他组分对NE测定的干扰，已用于实际样品NE含量的测定，结果令人满意。
关键词：聚伊文思蓝；修饰电极；电化学行为；循环伏安；去甲肾上腺素(NE)
中图分类号：R917&&& 文献标识码：A&& &文章编号：08)02-0247-04
Determination of norepinephrine in the presence of ascorbic acid with
poly Evans Blue modified glassy carbon electrode*
LIN Li-qing,YAO Hong,ZHUANG Qian,LI Wei,LIN Xin-hua **
（Department of Pharmaceutical Analysis,Faculty of Pharmacy,Fujian Medical University，Fuzhou 350004,China）
Abstract Objective:To study the electrochemical behavior of norepinephrine(NE) and ascorbic acid(AA)on the poly Evans Blue film modified electrode by cyclic voltammetry(CV) and establish a novel method for the determination of the content of NE.Method:The electrochemical behavior of NE and AA at the poly Evans Blue film modified electrode was studied by cyclic voltammetry while the content of NE was measured in differential pulse voltammetry(DPV).Results:The modified electrode shows enhanced sensitivity and excellent electrochemical discrimination to NE and AA,the oxidation potential difference of NE and AA was about 282 mV.In pH 5.0 phosphate buffer solution,the relationship between oxidation peak current and the concentration of NE was linear in the range of 5.0×10-7-1.8×10 -5 mol?L-1.The detection limit was 4.0×10-8 mol?L-1.Conclusion:Norepinephrine could be determined in the presence of ascorbic acid and the interference of other components can be efficiently eliminated on the modified electrode.This method can be used for the determination of NE in real sample with satisfactory results.
Key words：poly Evans Blue；modified electrode；electrocatalytic behavior；cyclicnorepinephrine(NE)
关于线性回归法与单点外标法测量不确定度评估的初步探讨
陈华，王慧
第一作者Tel：(010);E-mail:chenhua@
(中国药品生物制品检定所，北京 100050)
摘要目的：建立线性回归法与单点外标法的测量不确定度的评估方法，并进行比较。方法：分别采用线性回归法与单点外标法对同一批枸橼酸坦度螺酮片进行含量测定，并对结果进行评估。结果：线性回归法含量的测量不确定度评估结果为4.78%，单点外标法含量的测量不确定度评估结果为1.46%。结论：单点外标法比线性回归法有更小的测量不确定度。
关键词：测量不确定度；线性回归法；单点外标法
中图分类号：R917&& &文献标识码：A&&& 文章编号：08)02-0251-05
Preliminary discuss on the estimation of the uncertainty
measurement of linear regression method (LRM) and single
point external standard method(SPESM)
CHEN Hua,WANG Hui
(National Institute for the Control of Pharmaceutical and Biological
Products,Beijing 100050,China)
AbstractObjective:To establish methods to estimate the measurement uncertainty of linear regression method(LRM) and single point external standard method(SPESM).Method:Determining the content of the same batch of tandospirone citrate tablets with LRM and SPESM,then estimating their uncertainty.Result:The results of LRM and SPESM were 4.78% and 1.46% respectively.Conclusion:The uncertainty of SPESM is less than that of LEM.
Key words:measurementlinesingle point external standard method
内蒙古赤芍化学成分的HPLC-DAD/ESI-MS分析
沈陶冶1，张国兵1，吕佳妮2
通讯作者Tel:(2;E-mail:
（1.浙江大学医学院附属第一医院，杭州 310003；2.浙江省中医院，杭州 310006)
摘要 目的：利用液-质联用技术定性分析内蒙古赤芍药材中的化学成分。方法：以甲醇回流提取内蒙古赤芍药材。高效液相色谱条件：色谱柱为Zorbax SB-C18柱 (4.6 mm×250 mm，5 μm)，流动相0.2%的醋酸水溶液（A）-0.2%醋酸乙腈溶液（B），梯度洗脱,流速0.5 mL?min-1，柱温30 °C，二极管阵列检测器(DAD)，检测波长230 nm。质谱条件:负离子模式扫描，扫描范围 100~2000 amu；氮气流速10 L?min-1，雾化温度350 ℃，毛细管电压3500 V,裂解电压100 V。结果：通过高效液相色谱将赤芍化学成分较好地分离，根据紫外光谱可大致判断其化合物类型,由电喷雾质谱得到各成分的相对分子质量,进而推测出其中13个主要成分的可能结构。结论：液-质联用技术能快速定性研究赤芍药材中的化学成分，为赤芍指纹图谱的优化和质量标准的制定提供依据。
关键词：赤芍;化学成分;液-质联用
中图分类号：R917&&& 文献标识码：A&&& 08)02-0256-04
Analysis on chemical constituents of Paeonia& lactiflora Pall.
produced in Inner Mongolia by HPLC-DAD/ESI-MS
SHEN Tao-ye1,ZHANG Guo-bing1,La Jia-ni2*
（1.The First Affiliated Hospital,College of Medicine,Zhejiang University,Hangzhou .Zhejiang Hospital of Traditional Chinese Medicine,Hangzhou 310006,China)
Abstract Objective:To analyze the chemical constituents of Paeonia lactiflora Pall.by high performance liquid chromatography-diode array detector electrospray ionization-mass spectrometry (HPLC-DAD/ESI-MS).Method:The samples were extracted under reflux with methanol.The chromatographic separation was performed on a Zorbax SB-C18 column (4.6 mm×250 mm，5 μm)with a linear gradient elution of acetic acid-water (0.2∶100,v/v) and acetic acid-acetonitrile (0.2∶100,v/v).The flow rate was 0.5 mL?min-1 and column temperature was set at 30 ℃.The UV detection wavelength was set at 230 nm.The negative ionization mode,temperature of the capillary,350 ℃,capillary voltage,3500 V;gas (N2) flow,10 L?min-1,fragment voltage,100 V.Relative molecular mass data acquisition was performed from m/z 100 to 2000 in full MS scan mode.Result:The chemical constituents of Paeonia lactiflora Pall.were well isolated by HPLC，thirteen of the major chemical constituents were identified by the ESI-MS and ultraviolet (UV) spectra.Conclusion:HPLC-DAD/ESI-MS technology can be applied to study the chemical constituents,optimized the characteristic fingerprint and quality control method for this herb.
Key words: Paeonia lactiflora Pall.;chemicalHPLC-DAD/ESI-MS
RP-HPLC测定酸浆药材中3种有效成分的含量
施蕊，贾凌云，孙启时
通讯作者Tel:(024);E-mail:.cn,于丹丹
（沈阳药科大学中药学院，沈阳 110016）
摘要 目的：采用RP-HPLC建立同时测定酸浆药材中酸浆苦味素A、酸浆苦味素D及木犀草素含量的方法。方法：分析柱采用Diamonsil C18（200 mm×4.6 mm,5 μm）色谱柱，流动相为甲醇-0.2%醋酸（45∶55，v/v）；流速：1.0 mL?min-1；检测波长：220 nm。结果：酸浆苦味素A、酸浆苦味素D及木犀草素浓度分别在0.15~1.20 mg?mL-1 (r=0.9995)，0.10~0.81 mg?mL-1 (r=0.9996)，0.12~0.96 mg?mL-1 (r=0.9997)范围内与峰面积呈良好的线性关系，酸浆苦味素A平均回收率分别为95.9%，97.1%,103%；RSD分别为2.0%，0.7%，1.4%。酸浆苦味素D的平均回收率分别为97.3%，101%，97.1%；RSD分别为1.0%，1.9%，1.3%。木犀草素的平均回收率分别为97.8%，97.8%，97.7%；RSD分别为0.4%，2.9%，0.5%。结论：采用RP-HPLC 同时测定酸浆药材中酸浆苦味素A、酸浆苦味素D及木犀草素3种成分的含量，该法简单、可靠，可作为控制酸浆药材质量的参考标准。
关键词：酸浆；酸浆苦味素A；酸浆苦味素D；木犀草素；RP-HPLC
中图分类号：R917&&& 文献标识码：A&&& 文章编号：08)02-0260-03
RP-HPLC determination of there active components in
Physalis alkekengi L.var. franchetii (Mast.) Makino
SHI Rui，JIA Ling-yun，SUN Qi-shi*，YU Dan-dan
(Shenyang Pharmaceutical University,Shenyang 110016,China)
Abstract Objective:To establish a method for determination of physalin A,physalin D,and luteolin in Physalis alkekengi L. by RP-HPLC.Method:The sample was separated on Diamonsil C18（200 mm×4.6 mm,5 μm）column,the mobile phase was methanol-0.2% acetic acid (45∶55,v/v) at a flow rate of 1.0 mL?min-1 and the detection wavelength was 220 nm.Results:The linear range of physalin A,physalin D,and luteolin were 0.15-1.20 mg?mL-1 (r=0.-0.81 mg?mL-1 (r=0.-0.96 mg?mL-1 (r=0.9997),respectively.The average recoveries of physalin A were 95.9%，97.1% and 103%， RSD were 2.0%，0.7% and 1.4%； The average recoveries of physalin D were 97.3%，101% and 97.1%，RSD were 1.0%，1.9% and 1.3%； The average recoveries of luteolin were 97.8%，97.8% and 97.7%，RSD were 0.4%，2.9% and 0.5%.Conclusion:The method is simple,accurate,reproducible and can offer references for the quality control of Physalis alkekengi L.
Key words: Physalis alkekengi L.;physalin A;physalin D;RP-HPLC
不同方法提取的蓝布正挥发油的化学成分研究
张怡莎1，2，周欣1通讯作者Tel:（0851）6690018;E-mail:，
陈华国1，赵超1，刘海1，李章万3
(1.贵州师范大学天然药物质量控制研究中心，贵阳 .贵阳中医学院药学系，贵阳 550002;
3.四川大学华西药学院，成都 610041 )
摘要 目的：对3种不同方法提取的蓝布正挥发油的化学成分进行分析研究。方法：采取水蒸气蒸馏(SD)法、同时蒸馏萃取(SDE)法和微波萃取(MAE)法3种方法提取蓝布正挥发油，用GC-MS分析其化学成分。以HP-5MS毛细管柱为分离柱，程序升温从50 ℃（保持2 min）开始以4 ℃? min-1升到180 ℃，再以9 ℃? min-1升到290 ℃，保持5 min，气化室温度250 ℃，载气为高纯氦气(1.0 mL? min-1)。结果：通过计算机检索，共鉴定出58个化合物。结论：SD法和SDE法提取的挥发油成分相似，MAE法与前2种方法提取的挥发油化学成分有差异。
关键词：蓝布正；挥发油；水蒸气蒸馏(SD)；同时蒸馏萃取(SDE)；微波萃取(MAE)；GC-MS
中图分类号：R917&&& 文献标识码：A&&& 文章编号：08)02-0263-04
Analysis of chemical constituents of volatile oils from
Herba Gei with different extraction methods
ZHANG Yi-sha1,2，ZHOU Xin1*，CHEN Hua-guo1，ZHAO Chao1，LIU Hai1，LI Zhang-wan3
(1.The Research Center of Quality Control of Natural Medicines,Guizhou Normal University,Guiyang .Department of Pharmacy Guiyang College of TCM,Guiyang .West
&China School of Pharmacy,Sichuan University Department of Pharmacology,Chengdu 610041,China）
Abstract Objective:To analyze the chemical constituents of volatile oils from Herba Gei with three kinds of extraction methods.Methods:The volatile oils from Herba Gei were extracted by stream distillation(SD),simultaneous distillation extraction(SDE) and microwave extraction (MAE)method,and analyzed their spectrometry(GC-MS) by capillary columns gas chromatography with HP-5MS phenyl methyl siloxane capillary columns.The column temperature was in rate of 4 ℃? min-1 from 50 ℃ (hold 2 min) to 180 ℃,then in rate of 9 ℃? min-1& from 180 ℃ to 290 ℃(kept 5 min).The carrying gas was helium (1.0 mL? min-1).Results:58 compounds were identified.Conclusion:The compounds from the volatile oils extracted with SD and SDE are resemble.The oil with MAE is different from the two formers.
Key words:Herba Gei；volatile oils；stream distillation(SD);simultaneous distillation extraction(SDE)；microwave extraction(MAE)；GC-MS
顶空毛细管气相法测定鸡肝散提取物中有机溶剂残留量
浙江省自然科学基金(302682)；教育部高等学校博士学科点专项科研基金()；
浙江省科技厅基金(2004C33009)[浙江省中药现代化专项基金(浙财建字(号)]
王翰华，王向军，曾苏，姚彤炜通讯作者Tel：（0571）；E-mail：
（浙江大学药学院药物分析与药物代谢教研室，杭州 310058）
摘要 目的：建立鸡肝散提取物中3种有机溶剂残留量的测定方法。方法：用HP-5毛细管气相色谱柱，顶空进样，FID检测器，以标准溶液加入法进行计算。结果：乙醇、乙酸乙酯、正丁醇的线性范围分别为12.98~129.8 μg?mL-1(r=0.9996)，21.60~216.0 μg?mL-1(r=0.9993)，62.70~~627.0 μg?mL-1(r=0.9994)，回收率95.81%~104.2%，理论板数均大于13000，相邻峰的分离度均大于2，精密度、回收率RSD均小于10%。结论：本方法简单、准确，灵敏度高、重现性好，适用于鸡肝散提取物中有机溶剂残留量的测定。
关键词：鸡肝散提取物；顶空进样法；毛细管气相色谱法；有机溶剂残留量；标准溶液加入法
中图分类号：R917&&& 文献标识码：A&&& 文章编号：08)02-0267-03
Determination of residual organic solvents in Elsholtzia blanda
extracts by capillary gas chromatography with headspace sampling*
WANG Han-hua，WANG Xiang-jun，ZENG Su，YAO Tong-wei**
（Department of Pharmaceutical Analysis and Drug Metabolism,College of Pharmaceutical Sciences,
Zhejiang University，Hangzhou 310058,China）
AbstractObjective:To develope headspace gas chromatography method for the determination of residual organic solvents in Elsholtzia blanda extracts.Methods:The samples were injected into HP-5 capillary column by headspace sampler and analysed with FID detector with standard addition method.Results:The linear ranges of ethanol,ethyl acetate and nbutanol were 12.98-129.8 μg?mL-1(r=0.-216.0 μg?mL-1(r=0.9993) and 62.70-627.0 μg?mL-1(r=0.9994).The rate of recovery was in the range of 95.81%-104.2%.The numbers of theoretical plates were more than 13000 and the resolutions between the adjacent peaks were more than 2.The RSD of precision and accuracy were all less than 10%.Conclusions:The method is simple accurate and sensitive with good reproducibility.It can be used for the determination of the residual organic solvents in Elsholtzia blanda extracts.
Key words:Elsholtziacapillarresidstandard addition method
保健食品微生物限度检查的方法学验证
特玉香1，古丽巴哈尔托乎提2，杨洪淼1，刘岚3，马仕洪1，胡昌勤1
通讯作者Tel：(010)；Email:hucq@
（1.中国药品生物制品检定所，北京 100050；2.新疆维吾尔族自治区药品检验所，乌鲁木齐 830002；
3.湖南省衡阳市药品检验所，衡阳 421200）
摘要 目的：确认对保健食品进行微生物限度检查时，所采用的细菌、霉菌及酵母菌计数和控制菌检查方法是否适合于该保健食品的微生物限度检查。方法：按2005年版中国药典微生物限度检查法及方法学验证实验要求，对21种保健食品进行了方法学验证。结果：10个品种（血尔口服液、金舒通胶囊、事轻松胶囊、梦玉胶囊等）分别对金黄色葡萄球菌和枯草芽孢杆菌有明显的抑菌作用，阳性对照菌回收率均低于70%。结论：保健食品采用GB/T4789―2003食品卫生微生物学检查法进行检查时，其检验结果可能不够科学，建议参照2005年版中国药典要求，通过方法验证实验建立合理的检验方法。
关键词：方法学验证；微生物限度；回收率；保健食品质量
中图分类号：R917&&& 文献标识码：A&&& 文章编号：08)02-0270-05
Validation of method in microbial limit tests for health foods
TE Yu-xiang1,Gulibahaer Tuohuti2,YANG Hong-miao1,
LIU Lan3,MA Shi-hong1,HU Chang-qin1*
(1.National Institute for the Control of Pharmaceutical and Biological Products,Beijing 100050,China;
2.Xinjiang Provincial Institute for Drug Control,Wulumuqi 830002,China;
3.Hengyang Institute for Drug Control,Hengyang 421200,China)
Abstract Objective:To confirm that if the methods of total aerobic microbial count and absence bacteria test were appropriate in microbial limit tests for health foods.Methods:According to the Chinese Pharmacopoeia 2005,validated the microbiological test method of 21 kinds of health foods.Result:10 kinds of health care products (Xueer oral solution,Jinshutong capsule,Shiqingsong capsule and Mengyu capsule.etc.) were antibacterial for Staphylococcus aureus and Bacillus subtilis.The average recoveries were below to 70%.Conclusion:The method in foods microbial limit tests GB/T were not suitable for the microbial limit tests of health foods.It should set up more reasonable methods with validation according to the Chinese Pharmacopoeia 2005.
Key words:validation；microbial limits；recovery rate；quality of health foods
注射用奥美拉唑钠细菌内毒素检查法
潘正兴,宋勤
第一作者Tel: (, ;E-mail：
（贵州省药品检验所，贵阳 550004）
摘要 目的：对注射用奥美拉唑钠进行凝胶法干扰试验，建立注射用奥美拉唑钠细菌内毒素检查的试验方法。方法：采用2005年版中国药典二部附录细菌内毒素检查法。结果：注射用奥美拉唑钠稀释5倍（2 mg?mL-1）时对细菌内毒素检查法无干扰作用。结论：使用细菌内毒素检查法检查注射用奥美拉唑钠中的细菌内毒素是可行的，可用细菌内毒素检查法代替家兔热原检查法。
关键词：注射用奥美拉唑钠；细菌内毒素；凝胶法；干扰试验
中图分类号：R917&&& 文献标识码：A&&& 文章编号：08)02-0275-03
Study on determination of bacterial endotoxin of
omeprazole sodium for injection
PAN Zheng-xing,SONG Qin
(Guizhou Institute for Drug Control,Guiyang 550004,China)
Abstract Objective:To establish a method for the determination of bacterial endotoxin of omeprazole Method:According to the method of determination of bacterial endotoxin approved by Chinese Pharmacopoeia 2005 edition.Results:The interference on the determination of bacterial endotoxin can be excluded when omeprazole sodium for injection was diluted 5 times.Conclusion:It is feasible to detect the bacterial endotoxin of omeprazole sodium for injection by the method of determination of bacterial endotoxin and the method may replace pyrogen test.
Key words:omeprazole Gelation Ainhibition or enhancement test
田七痛经胶囊检测方法的研究
梁懿，蒙连琼
第一作者Tel：(7；E-mail：
（广西南宁百会药业集团有限公司药物研究所，南宁530003）
摘要 目的：建立田七痛经胶囊的质量控制方法。方法：采用TLC方法对田七痛经胶囊中的木香、川芎、延胡索进行定性鉴别；采用HPLC法，YWG C18色谱柱（250 mm×4.6 mm，10 μm），以乙腈-0.05%（v/v）磷酸溶液（100∶400）为流动相，流速1 mL?min-1，检测波长203 nm，柱温为室温，进样量20 μL，对田七痛经胶囊中的三七皂苷R1、人参皂苷Rg1和人参皂苷Re进行定性鉴别，并对人参皂苷Rg1进行含量测定。结果：木香、川芎、延胡索的薄层鉴别和三七皂苷R1、人参皂苷Rg1和人参皂苷Re的HPLC鉴别专属性强，人参皂苷Rg1进样量在3.0~15.0 μg范围内与峰面积呈良好的线性关系（r=1.000，n=5）。人参皂苷Rg1平均回收率为99.1%，RSD=2.6%（n=5）。结论：本方法可准确地进行定性、定量，可用于控制田七痛经胶囊的质量。
关键词：田七痛经胶囊；人参皂苷Rg1；含量测定；高效液相色谱法
中图分类号：R917&&& 文献标识码：A&&& 文章编号：08)02-0278-04
Study on the quality control standard of Tianqi Tongjing capsules
LIANG Yi，MENG Lian-qiong
(Institute of Pharmacology,Best & Wide Pharmaceutical Co.,Ltd.,Nanning Guangxi,Nanning 530003,China)
Abstract O bjective:To establish the quality control standard of Tianqi Tongjing capsules.Method:Radix Aucklandiae,Rhizoma Chuanxiong,Rhizoma Corydalis were identified by TLC.Notoginsenoside R1,ginsenoside Rg1,ginsenoside Re in Tianqi Tongjing capsules were identified and the content of ginsenoside Rg1 was determined by HPLC.YWG C18& column(250 mm×4.6 mm，10 μm) was adopted.The mobile phase was acetonitrile-0.05%(v/v) phosphoric acid (100∶400) at a flow rate of 1 mL?min-1 .The dete