CN101334386A - 扶正化淤植物药血浆苦杏仁苷的测定方法 - Google Patents
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Abstract
本发明涉及扶正化淤植物药血浆苦杏仁苷的测定方法,包括步骤:(1)将哺乳类给予扶正化淤植物药后的含药血浆,先加2-5mol/L磷酸混匀后,血浆与磷酸体积比为1∶2-3,加入已用甲醇和水活化后的waters Oasis HLB小柱,经水及80-100%甲醇淋洗和0.2-1%氨水甲醇洗脱后,洗脱液在25-30℃条件下挥干富集,用流动相复溶;(2)UPLC/MS法检测色谱条件:色谱柱:Acquity UPLC BEH C18,2.1×100mm,流动相A:Water-Acetonitrile-Formic acid 95∶5∶0.1v/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 150~800;本发明适合用于扶正化淤植物药苦杏仁苷的药代动力学研究。
Description
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苦杏仁苷的测定方法。
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)中苦杏仁苷的测定方法。
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苦杏仁苷的测定方法,该方法用于药代动力学研究,阐明扶正化淤植物药苦杏仁苷的药代动力学规律。
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苦杏仁苷的测定方法,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,先加2-5mol/L磷酸混匀后,血浆与磷酸体积比为1∶2-3,加入已用甲醇和水活化后的Waters Oasis HLB小柱,经水及80-100%甲醇淋洗和0.2-1%氨水甲醇洗脱后,洗脱液在25-30℃条件下挥干富集,用流动相复溶;
b.UPLC/MS法检测;
(2).UPLC/MS测定方法
色谱条件:色谱柱:Acquity UPLC BEH C18,2.1×100mm,流动相A:Water-Acetonitrile-Formic acid 95∶5∶0.1v/v/v,流动相B:Acetonitrile-Formic acid100∶0.1v/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 150~800。
所述步骤(2)电喷雾离子源,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 150~800。
本发明在固相萃取过程中,固相对分析物的吸附力大于样品母液,当样品通过固相萃取柱时,分析物及一些相近似的成分被吸附在固体表面,其他组分则随样品母液通过柱子,先用极性较大的溶剂淋洗柱子,将一些无关的成分清洗去除,最后用适当的溶剂将分析物洗脱下来,洗脱液抽干富集;利用UPLC系统,将分析物与洗脱液中的其他成分进行分离,最后通过质谱检测仪进行检测。
本发明的苦杏仁苷为水溶性成分,采用固相萃取方法,可充分将样品中的苦杏仁苷萃取出来,再加上使用UPLC/MS系统进行检测,使苦杏仁苷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苦杏仁苷的血药浓度测定。
附图说明
图1苦杏仁苷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苦杏仁苷测定方法包括:
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先加2.17mol/L磷酸混匀后,生物样品与磷酸之间的体积比为:1∶2-3;再加入已用甲醇和水活化后的WatersOasis HLB小柱,经水及80-100%甲醇淋洗和0.2-1%氨水甲醇洗脱后,洗脱液在25℃条件下挥干富集,用流动相复溶。
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:Acquity UPLCBEH C18,2.1×100mm,流动相A:Water-Acetonitrile-Formic acid 95∶5∶0.1v/v/v,流动相B:Acetonitrile-Formic acid 100∶0.1v/v,按下列梯度洗脱:
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 150~800。
测定结果:哺乳类灌服扶正化淤植物药后血浆中可测出苦杏仁苷(见图1).
Claims (2)
1、扶正化淤植物药血浆苦杏仁苷的测定方法,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,先加2-5mol/L磷酸混匀后,血浆与磷酸体积比为1∶2-3,加入已用甲醇和水活化后的Waters Oasis HLB小柱,经水及80-100%甲醇淋洗和0.2-1%氨水甲醇洗脱后,洗脱液在25-30℃条件下挥干富集,用流动相复溶;
b.UPLC/MS法检测;
(2).UPLC/MS测定方法
色谱条件:色谱柱:Acquity UPLC BEH C18,2.1×100mm,流动相A:Water-Acetonitrile-Formic acid 95∶5∶0.1v/v/v,流动相B:Acetonitrile-Formic acid100∶0.1v/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 150~800。
2.根据权利要求1所述的扶正化淤植物药血浆苦杏仁苷的测定方法,其特征在于:所述步骤(2)电喷雾离子源,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 150~800。
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EP08748426.7A EP2144058B1 (en) | 2007-04-27 | 2008-04-28 | Detection of blood plasma amygdalin of dissipating blood stasis botanical |
CA2685359A CA2685359C (en) | 2007-04-27 | 2008-04-28 | Method of detecting blood plasma amygdalin after administration of fuzheng huayu(fzhy) |
US12/451,148 US8334110B2 (en) | 2007-04-27 | 2008-04-28 | Detection of blood plasma amygdalin of dissipating blood stasis botanical |
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Cited By (3)
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CN109596745A (zh) * | 2018-12-28 | 2019-04-09 | 成都普思生物科技股份有限公司 | 一种高效液相色谱法在苦杏仁苷检测中的应用及特征图谱 |
CN110836934A (zh) * | 2019-11-22 | 2020-02-25 | 成都中医药大学 | 一种桃仁与光核桃仁分析模型的构建方法及鉴别应用 |
CN113189210A (zh) * | 2019-12-31 | 2021-07-30 | 上海黄海制药有限责任公司 | 测定血浆中苦杏仁苷、柚皮素、槲皮素浓度的hplc-ms/ms方法 |
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CN108267515B (zh) * | 2016-12-30 | 2020-10-02 | 广州中医药大学第一附属医院 | 一种检测待测物中d-苦杏仁苷和/或l-苦杏仁苷含量的方法 |
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CN113820420B (zh) * | 2021-09-23 | 2023-04-18 | 中国热带农业科学院热带作物品种资源研究所 | 一种采用uplc-q-tof-ms对益智酒中化学成分的测定方法 |
CN114755331B (zh) * | 2022-04-06 | 2024-04-12 | 重庆市食品药品检验检测研究院 | Uplc-q-tof法鉴别舒筋活血丸中6种组分的方法 |
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JPH01165583A (ja) | 1987-12-23 | 1989-06-29 | Tsumura & Co | (+)‐(6S,7S,R‐biar)‐5,6,7,8‐テトラヒドロ‐1,2,3,12‐テトラメトキシ‐6,7‐ジメチル‐10,11‐メチレンジオキシ‐6‐ジベンゾ[a,c]シクロオクテノールの製造方法 |
CN1069542C (zh) | 1999-07-19 | 2001-08-15 | 上海中医药大学 | 一种治疗慢性肝病的药物及其制备方法 |
KR100344751B1 (ko) | 1999-12-08 | 2002-07-20 | 주식회사 삼양제넥스 | 멜라닌 합성 저해물질 및 그것을 함유하는 조성물 |
CN1218745C (zh) | 2002-07-12 | 2005-09-14 | 上海现代中医药技术发展有限公司 | 一种保肝护肝及调节血脂的保健食品及其制备方法 |
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KR100510885B1 (ko) * | 2002-08-12 | 2005-08-26 | (주) 한약마을 | 아미그달린과 네오아미그달린의 역상 고성능 액체크로마토그래피 분리법 개발 및 아미그달린의 라세미화억제를 위한 최적 조건을 얻는 방법 |
CN1228070C (zh) * | 2002-12-27 | 2005-11-23 | 李晓恩 | 一种治疗肝纤维化及早期肝硬化的中药制剂 |
CN1511574A (zh) * | 2002-12-31 | 2004-07-14 | 中国中医药科技开发交流中心 | 一种防治肝纤维化的药物组合物及其制备方法 |
GB2411114B (en) | 2004-02-19 | 2006-08-16 | Phynova Ltd | A botanical drug or dietary supplement |
CN100450501C (zh) | 2004-03-17 | 2009-01-14 | 天津天士力制药股份有限公司 | 一种治疗心脑血管疾病的中药制剂及其制备方法 |
KR20060038027A (ko) * | 2004-10-29 | 2006-05-03 | (주) 한약마을 | 도인 또는 행인으로부터 아미그달린을 효과적으로 얻는추출방법 및 hplc를 이용한 분리방법 |
GB2428974B (en) | 2005-08-12 | 2010-02-03 | Phynova Ltd | Further medical use of a botanical drug or dietary supplement |
CN100594206C (zh) | 2005-08-19 | 2010-03-17 | 华东理工大学 | 从丹参中提取原儿茶醛和丹参酚酸的方法 |
CN100392400C (zh) | 2005-11-01 | 2008-06-04 | 上海中医药大学 | 生物体液中丹酚酸b浓度测定样品的预处理方法 |
CN1839996A (zh) * | 2006-01-12 | 2006-10-04 | 上海现代中医药技术发展有限公司 | 一种治疗慢性肝病的中药复方制剂及其制备方法 |
CN101040907B (zh) | 2007-04-27 | 2011-01-05 | 上海现代中医药技术发展有限公司 | 扶正化瘀植物药中丹参原料指纹图谱质量检测方法 |
CN101078712A (zh) * | 2007-04-27 | 2007-11-28 | 上海现代中医药技术发展有限公司 | 扶正化瘀植物药血浆丹参素和丹酚酸b的测定方法 |
CN101042380A (zh) * | 2007-04-27 | 2007-09-26 | 上海现代中医药技术发展有限公司 | 扶正化淤植物药血浆五味子乙素的测定方法 |
CN100573140C (zh) | 2007-04-29 | 2009-12-23 | 上海现代中医药技术发展有限公司 | 扶正化瘀植物药中五味子原料指纹图谱质量检测方法 |
CN101045092A (zh) * | 2007-04-29 | 2007-10-03 | 上海现代中医药技术发展有限公司 | 一种扶正化瘀植物药组合物的应用 |
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Cited By (3)
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CN109596745A (zh) * | 2018-12-28 | 2019-04-09 | 成都普思生物科技股份有限公司 | 一种高效液相色谱法在苦杏仁苷检测中的应用及特征图谱 |
CN110836934A (zh) * | 2019-11-22 | 2020-02-25 | 成都中医药大学 | 一种桃仁与光核桃仁分析模型的构建方法及鉴别应用 |
CN113189210A (zh) * | 2019-12-31 | 2021-07-30 | 上海黄海制药有限责任公司 | 测定血浆中苦杏仁苷、柚皮素、槲皮素浓度的hplc-ms/ms方法 |
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WO2008131649A1 (en) | 2008-11-06 |
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US8334110B2 (en) | 2012-12-18 |
CN101334386B (zh) | 2012-07-11 |
US20100173345A1 (en) | 2010-07-08 |
CA2685359A1 (en) | 2008-11-06 |
EP2144058A4 (en) | 2010-05-26 |
EP2144058B1 (en) | 2015-06-10 |
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