首页|UPLC-MS/MS法同时测定比格犬血浆中表儿茶素与4β-(2-氨基乙硫基)表儿茶素

UPLC-MS/MS法同时测定比格犬血浆中表儿茶素与4β-(2-氨基乙硫基)表儿茶素

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目的:建立UPLC-MS/MS法同时测定比格犬血浆中表儿茶素(EC)与4β-(2-氨基乙硫基)表儿茶素(Cya-EC)的浓度,研究比格犬口服威麦宁胶囊后体内药代动力学.方法:血浆样品经盐酸巯乙胺衍生化处理后,以乙腈-水(0.1%甲酸)为流动相梯度洗脱,Waters BEH Shield RP18(100 mm×2.11 mm,1.7 μm)色谱柱分离,采用电喷雾电离源,以多反应监测方式进行正离子检测,定量分析所用的离子反应分别为m/z 291.1→138.9(EC)、m/z 366.1→288.9(Cya-EC)和m/z 260.2→116.3(内标:普萘洛尔).结果:测定血浆中EC及Cya-EC的线性范围均为10 ~ 2000 ng·mL-1,日内、日间精密度均小于14.82%,准确度均在±4.86%以内;使用DAS3.0药代动力学软件对血药浓度数据进行处理,计算药动学参数,EC及Cya-EC的主要药动学参数t1/2分别为66.3和90.4h,AUC0-∞分别为2 114.7和12 909.5 ng·h·mL@-1.结论:本文建立的UPLC-MS/MS法运行时间短、选择性强、灵敏度高、操作简便、血浆用量少,适用于比格犬口服威麦宁胶囊后体内EC及Cya-EC的药代动力学研究.
Simultaneous Determination of Epicatechin and 4β-2(aminoethylthio)Epicatechin in Dog Plasma by UPLC-MS/MS
Objective:To establish a sensitive and rapid liquid chromatography-tandem mass spectrometry(LC-MS/MS)method to simultaneously determinate epicatechin(EC)and 4β-2(aminoethylthio)epicatechin(Cya-EC)in plasma of beagle dogs after oral administration of WeiMaiNing capsule.Method:Chromatographic separation was achieved on an Waters BEH Shield RP18(100 mm×2.1 mm,1.7 μm)using a step gradient program with the mobile phase of 0.1% formic acid aqueous solution and acetonitrile with 0.1% formic acid,at a flow-rate of 0.30 mL-1.Electrospray ionization(ESI)source was applied and operated in the positive ion mode.Multiple reaction monitoring mode with the transitions of m/z 291.1→138.9(EC),m/z 366.1→288.9(Cya-EC)and m/z 260.2→116.3(IS,propranolol)was performed to quantify,respectively.Results:The linear concentration ranges of calibration curves for EC and Cya-EC were 10-2000 ng·mL-1.The inter-or intra-day precision(RSD)was less than 14.82%,and the accuracy(RE)was within±4.86%.The pharmacokinetic parameters were calculated by DAS3.0.The t1/2 of EC and Cya-EC were 66.3 and 90.4 h.And the AUC0-∞ of EC and Cya-EC were 2 114.7 and 12 909.5 ng·h·mL-1 in beagle dog plasma after oral administration of WeiMaiNing capsules.Conclusion:The method was sensitive,rapid,convenient,using less plasma and was proved to be suitable for preclinical pharmacokinetic studies of EC and Cya-EC in beagle dog after oral administration of Wei MaiNing capsules.

Epicatechin4β-2(aminoethylthio)epicatechinUPLC-MS/MSdog plasma

戴玮、付淑军、常新全、王鹏、郝彧、左臣强、石小娜、何新

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中国中药公司,北京 100195

天津中医药大学 中药学院,天津 300193

天津市创新药物早期成药性评价企业重点实验室(筹),天津 300457

瀚盟测试科技(天津)有限公司,天津 300457

天津国际生物医药联合研究院,天津 300457

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表儿茶素 4β-(2-氨基乙硫基)表儿茶素 超高效液相色谱-串联质谱 比格犬血浆 威麦宁胶囊

中国医药集团新产品开发基金

2011ZY01

2017

中国现代中药
中国中药协会,中国医药集团总公司,中国药材公司

中国现代中药

CSTPCD
影响因子:0.65
ISSN:1673-4890
年,卷(期):2017.19(3)
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