CN101042380A - 扶正化淤植物药血浆五味子乙素的测定方法 - Google Patents

扶正化淤植物药血浆五味子乙素的测定方法 Download PDF

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CN101042380A
CN101042380A CN200710040140.1A CN200710040140A CN101042380A CN 101042380 A CN101042380 A CN 101042380A CN 200710040140 A CN200710040140 A CN 200710040140A CN 101042380 A CN101042380 A CN 101042380A
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schizandrin
uplc
acetonitrile
plasma
voltage
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马越鸣
石荣
张永煜
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SHANGHAI MODERN CHINESE TRADITIONAL MEDICINE TECHNOLOGY DEVELOPMENT Co Ltd
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SHANGHAI MODERN CHINESE TRADITIONAL MEDICINE TECHNOLOGY DEVELOPMENT Co Ltd
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Priority to CN200710040140.1A priority Critical patent/CN101042380A/zh
Publication of CN101042380A publication Critical patent/CN101042380A/zh
Priority to CA2685357A priority patent/CA2685357C/en
Priority to US12/451,141 priority patent/US7989212B2/en
Priority to EP08748424.2A priority patent/EP2146206B1/en
Priority to PCT/CN2008/000865 priority patent/WO2008131647A1/zh
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    • G—PHYSICS
    • G01—MEASURING; TESTING
    • G01N—INVESTIGATING OR ANALYSING MATERIALS BY DETERMINING THEIR CHEMICAL OR PHYSICAL PROPERTIES
    • G01N33/00—Investigating or analysing materials by specific methods not covered by groups G01N1/00 - G01N31/00
    • G01N33/48—Biological material, e.g. blood, urine; Haemocytometers
    • G01N33/50—Chemical analysis of biological material, e.g. blood, urine; Testing involving biospecific ligand binding methods; Immunological testing
    • G01N33/94—Chemical analysis of biological material, e.g. blood, urine; Testing involving biospecific ligand binding methods; Immunological testing involving narcotics or drugs or pharmaceuticals, neurotransmitters or associated receptors
    • G—PHYSICS
    • G01—MEASURING; TESTING
    • G01N—INVESTIGATING OR ANALYSING MATERIALS BY DETERMINING THEIR CHEMICAL OR PHYSICAL PROPERTIES
    • G01N33/00—Investigating or analysing materials by specific methods not covered by groups G01N1/00 - G01N31/00
    • G01N33/48—Biological material, e.g. blood, urine; Haemocytometers
    • G01N33/50—Chemical analysis of biological material, e.g. blood, urine; Testing involving biospecific ligand binding methods; Immunological testing
    • G01N33/94—Chemical analysis of biological material, e.g. blood, urine; Testing involving biospecific ligand binding methods; Immunological testing involving narcotics or drugs or pharmaceuticals, neurotransmitters or associated receptors
    • G01N33/9453—Cardioregulators, e.g. antihypotensives, antiarrhythmics
    • Y—GENERAL TAGGING OF NEW TECHNOLOGICAL DEVELOPMENTS; GENERAL TAGGING OF CROSS-SECTIONAL TECHNOLOGIES SPANNING OVER SEVERAL SECTIONS OF THE IPC; TECHNICAL SUBJECTS COVERED BY FORMER USPC CROSS-REFERENCE ART COLLECTIONS [XRACs] AND DIGESTS
    • Y10—TECHNICAL SUBJECTS COVERED BY FORMER USPC
    • Y10T—TECHNICAL SUBJECTS COVERED BY FORMER US CLASSIFICATION
    • Y10T436/00—Chemistry: analytical and immunological testing
    • Y10T436/20—Oxygen containing
    • Y10T436/203332—Hydroxyl containing
    • Y—GENERAL TAGGING OF NEW TECHNOLOGICAL DEVELOPMENTS; GENERAL TAGGING OF CROSS-SECTIONAL TECHNOLOGIES SPANNING OVER SEVERAL SECTIONS OF THE IPC; TECHNICAL SUBJECTS COVERED BY FORMER USPC CROSS-REFERENCE ART COLLECTIONS [XRACs] AND DIGESTS
    • Y10—TECHNICAL SUBJECTS COVERED BY FORMER USPC
    • Y10T—TECHNICAL SUBJECTS COVERED BY FORMER US CLASSIFICATION
    • Y10T436/00—Chemistry: analytical and immunological testing
    • Y10T436/24—Nuclear magnetic resonance, electron spin resonance or other spin effects or mass spectrometry

Abstract

本发明涉及扶正化淤植物药血浆五味子乙素的测定方法。包括：(1)将哺乳类给予扶正化淤植物药后的含药血浆，用1∶4体积比加乙酸乙酯进行萃取，涡旋3－5分钟，9600rpm离心10分钟，上层在25－30℃条件下挥干富集，用流动相复溶；(2)UPLC/MS测定：色谱条件：色谱柱：Acquity UPLC BEH C18，2.1×100mm，流动相A：Water－Acetonitrile－Formic acid 95∶5∶0.1 v/v/v，流动相B：Acetonitrile－Formic acid100∶0.1 v/v；质谱条件：电喷雾离子源(ESI)，采用正离子模式检测，质量扫描范围m/z 150～1200。本发明适合用于扶正化淤植物药五味子乙素的药代动力学研究。

Description

扶正化淤植物药血浆五味子乙素的测定方法
技术领域
本发明属药物代谢动力学领域，特别是涉及扶正化淤植物药血浆五味子乙素的测定方法。
背景技术
扶正化淤植物药由丹参、桃仁、五味子等复方组成，具有治疗肝、肺、肾纤维化的作用，但对扶正化淤植物药缺乏药物代谢动力学的研究，因而对体内的药效成分不清楚，难以为质量控制及指导临床合理用药提供依据，阻碍了该药进入国际市场。
到目前为止，未见有关扶正化淤植物药药物代谢动力学的研究报道，无该复方在生物样品(包括血浆样品)中五味子乙素的测定方法。
发明内容
本发明所要解决的技术问题是提供扶正化淤植物药血浆五味子乙素的测定方法，该方法用于药代动力学研究，阐明扶正化淤植物药五味子乙素的药代动力学规律。
本发明解决的技术问题通过以下技术方案来实现：
扶正化淤植物药血浆五味子乙素的测定方法，包括下列步骤：
(1)哺乳类血浆样品预处理
a.将动物给予扶正化淤制剂后的含药血浆用1∶4加乙酸乙酯进行萃取，涡旋3-5分钟，9600rpm离心10分钟，上层在25-30℃条件下挥干富集；
b.流动相复溶后用UPLC/MS分析；
(2)UPLC/MS测定
色谱条件：色谱柱：Acquity UPLC BEH C18，2.1×100mm，流动相A：Water-Acetonitrile-Formic acid  95∶5∶0.1 v/v/v，流动相B：Acetonitrile-Formic acid100∶0.1 v/v；质谱条件：电喷雾离子源(ESI)，采用正离子模式检测，质量扫描范围m/z 150～1200。
所述步骤(2)采用正离子模式检测；脱溶剂气流量为440L/h，脱溶剂气温度为300℃，锥孔气流量为50L/h，离子源温度为100℃，喷雾毛细管电压为3800V，取样锥孔电压为30V，萃取锥孔电压为2.00V，透镜电压0.1V。质量扫描范围m/z 150～1200。
本发明在液液萃取过程中，被测组分在不相混溶的两种溶剂中分配，选择合适的有机溶剂及合适的比例，可使溶于血浆中的非极性组分提取进入有机相，再将有机相抽干富集；利用UPLC系统，将分析物与其他成分进行分离，最后通过质谱检测仪进行检测。
本发明中采用的乙酸乙酯液液萃取方法可将血浆中的五味子乙素萃取出来，再加上使用UPLC/MS系统进行检测，使五味子乙素与样品中其他成分的分离度明显提高，且分析方法更加灵敏和快捷，以利于进行药代动力学研究中五味子乙素的血药浓度测定。
附图说明
图1五味子乙素UPLC-MS色谱图。
具体实施方式
下面结合具体实施例，进一步阐述本发明。应理解，这些实施例仅用于说明本发明而不用于限制本发明的范围。此外应理解，在阅读了本发明讲授的内容之后，本领域技术人员可以对本发明作各种改动或修改，这些等价形式同样落于本申请所附权利要求书所限定的范围。
                            实施例1
一种血浆中扶正化淤植物药的五味子乙素测定方法包括：
1、血浆样品预处理方法：将哺乳类给予扶正化淤植物药后的含药血浆按1∶4加乙酸乙酯进行萃取，涡旋3分钟，9600rpm离心10分钟，上层在25℃条件下挥干富集，流动相复溶后用UPLC/MS分析。
2、UPLC/MS测定方法：本发明采用UPLC/MS法的分析条件色谱条件：色谱柱：AcquityUPLC BEH C18，2.1×100mm，流动相A：Water-Acetonitrile-Formic acid 95∶5∶0.1 v/v/v，流动相B：Acetonitrile-Formic acid 100∶0.1 v/v，按下列梯度洗脱：
Time(min)     Flow Rate(mL/min) ％A ％B
    05.0010.0020.0030.0035.0035.0138.00     0.3000.3000.3000.3000.3000.3000.3000.300     10085.070.040.020.020.0100.0100.0     015.030.060.080.080.00.00.0
质谱条件：电喷雾离子源(ESI)，采用正离子模式检测；脱溶剂气流量为440L/h，脱溶剂气温度为300℃，锥孔气流量为50L/h，离子源温度为100℃，喷雾毛细管电压为3800V，取样锥孔电压为30V，萃取锥孔电压为2.00V，透镜电压0.1V。质量扫描范围m/z 150～1200。
测定结果：哺乳类灌服扶正化淤植物药后血浆中可测出五味子乙素(见图1)。

Claims (2)

1.扶正化淤植物药血浆五味子乙素的测定方法，包括下列步骤：
(1)哺乳类血浆样品预处理
a.将哺乳类给予扶正化淤植物药后的含药血浆，用1∶4体积比加乙酸乙酯进行萃取，涡旋3-5分钟，9600rpm离心10分钟，上层在25-30℃条件下挥干富集，用流动相复溶；
b.流动相复溶后用UPLC/MS分析。
(2)UPLC/MS测定
色谱条件：色谱柱：Acquity UPLC BEH C18，2.1×100mm，流动相A：Water-Acetonitrile-Formic acid  95∶5∶0.1 v/v/v，流动相B：Acetonitrile-Formic acid100∶0.1 v/v；质谱条件：电喷雾离子源(ESI)，采用正离子模式检测，质量扫描范围m/z 150～1200。
2.根据权利要求1所述的扶正化淤植物药血浆五味子乙素的测定方法，其特征在于：所述步骤(2)采用正离子模式检测；脱溶剂气流量为440L/h，脱溶剂气温度为300℃，锥孔气流量为50L/h，离子源温度为100℃，喷雾毛细管电压为3800V，取样锥孔电压为30V，萃取锥孔电压为2.00V，透镜电压0.1V。质量扫描范围m/z 150～1200。
CN200710040140.1A 2007-04-27 2007-04-27 扶正化淤植物药血浆五味子乙素的测定方法 Pending CN101042380A (zh)

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CN200710040140.1A CN101042380A (zh) 2007-04-27 2007-04-27 扶正化淤植物药血浆五味子乙素的测定方法
CA2685357A CA2685357C (en) 2007-04-27 2008-04-28 Method of detecting blood plasma schizandrin b after administration of fuzheng huayu (fzhy)
US12/451,141 US7989212B2 (en) 2007-04-27 2008-04-28 Detection of blood plasma schizadrin B of dissipating blood stasis botanical
EP08748424.2A EP2146206B1 (en) 2007-04-27 2008-04-28 Detection of blood plasma schizandrin b of dissipating blood stasis botanical
PCT/CN2008/000865 WO2008131647A1 (en) 2007-04-27 2008-04-28 Detection of blood plasma schizadrin b of dissipating blood stasis botanical

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WO2008131647A1 (en) * 2007-04-27 2008-11-06 Shanghai Sundise Chinese Medicine Technology Development Co., Ltd. Detection of blood plasma schizadrin b of dissipating blood stasis botanical
US7993928B2 (en) 2007-04-27 2011-08-09 Shanghai Sundise Detection of blood plasma Danshensu and Salvianolic acid B dissipating blood stasis botanical
US8334110B2 (en) 2007-04-27 2012-12-18 Shanghai Sundise Chinese Medicine Technology Development Co., Ltd. Detection of blood plasma amygdalin of dissipating blood stasis botanical
US9161959B2 (en) 2007-04-29 2015-10-20 Shanghai Sundise Chinese Medicine Technology Development Co., Ltd Use of a vegetable drug composition in the manufacturing of pharmaceutical preparation for the treatment of portal hypertension caused by hepatocirrhosis

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WO2008131647A1 (en) * 2007-04-27 2008-11-06 Shanghai Sundise Chinese Medicine Technology Development Co., Ltd. Detection of blood plasma schizadrin b of dissipating blood stasis botanical
US7989212B2 (en) 2007-04-27 2011-08-02 Shanghai Sundise Detection of blood plasma schizadrin B of dissipating blood stasis botanical
US7993928B2 (en) 2007-04-27 2011-08-09 Shanghai Sundise Detection of blood plasma Danshensu and Salvianolic acid B dissipating blood stasis botanical
US8334110B2 (en) 2007-04-27 2012-12-18 Shanghai Sundise Chinese Medicine Technology Development Co., Ltd. Detection of blood plasma amygdalin of dissipating blood stasis botanical
US9161959B2 (en) 2007-04-29 2015-10-20 Shanghai Sundise Chinese Medicine Technology Development Co., Ltd Use of a vegetable drug composition in the manufacturing of pharmaceutical preparation for the treatment of portal hypertension caused by hepatocirrhosis

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US7989212B2 (en) 2011-08-02
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EP2146206A1 (en) 2010-01-20
CA2685357C (en) 2016-02-09
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US20100093103A1 (en) 2010-04-15

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