CN105911187A - 液质串联检测妇康宁片中盐酸水苏碱含量的方法 - Google Patents

液质串联检测妇康宁片中盐酸水苏碱含量的方法 Download PDF

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CN105911187A
CN105911187A CN201610259400.3A CN201610259400A CN105911187A CN 105911187 A CN105911187 A CN 105911187A CN 201610259400 A CN201610259400 A CN 201610259400A CN 105911187 A CN105911187 A CN 105911187A
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ethanol
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stachydrine
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陈学松
陈江涛
梁慧敏
李亚
李澄
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Wuzhou Institutes for Food and Drug Control
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    • G01—MEASURING; TESTING
    • G01N—INVESTIGATING OR ANALYSING MATERIALS BY DETERMINING THEIR CHEMICAL OR PHYSICAL PROPERTIES
    • G01N30/00—Investigating or analysing materials by separation into components using adsorption, absorption or similar phenomena or using ion-exchange, e.g. chromatography or field flow fractionation
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    • G01N—INVESTIGATING OR ANALYSING MATERIALS BY DETERMINING THEIR CHEMICAL OR PHYSICAL PROPERTIES
    • G01N30/00—Investigating or analysing materials by separation into components using adsorption, absorption or similar phenomena or using ion-exchange, e.g. chromatography or field flow fractionation
    • G01N30/02—Column chromatography
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Abstract

本发明提供了一种液质串联检测妇康宁片中盐酸水苏碱含量的方法，旨在提供一种灵敏度高，定性定量准确的液质串联检测妇康宁片中盐酸水苏碱含量的方法；其该方法是：1)制备供试品溶液；2)制备阴性对照溶液；3)制备对照品溶液；4)分别称取供试品溶液、对照品溶液和阴性对照溶液，上Agilent1295‑6550C三重四级杆液相质谱联用仪检测；属于化学检测技术领域。

Description

液质串联检测妇康宁片中盐酸水苏碱含量的方法
技术领域
本发明提供一种测定盐酸水苏碱含量的方法，具体地说，是液质串联检测妇康宁片中盐酸水苏碱含量的方法；属于化学检测技术领域。
背景技术
妇康宁片处方由白芍、益母草、香附等八味中药组成，具有养血理气，活血调经的功效，主治血虚气滞所致的月经不调。方中益母草为中医妇科良药，属唇形科植物益母草(Leonurus iaponicusHoutt.)的新鲜或干燥地上部分，其性微寒，味苦、辛，具有活血调经，利水消肿，清热解毒之功效，用于月经不调，痛经经闭，恶露不尽，水肿尿少，疮肿毒。
妇康宁片收载于《中国药典》2010年版一部，其质量标准收载了方中君药白芍的含量测定方法，而其臣药益母草只有盐酸水苏碱的薄层鉴别方法。经查阅文献，未见报道测定妇康宁片中盐酸水苏碱的含量方法。
发明内容
针对上述不足，本发明的目的是提供一种灵敏度高，定性定量准确的液质串联检测妇康宁片中盐酸水苏碱含量的方法。
为解决上述技术问题，本发明提供的技术方案如下：
一种液质串联检测妇康宁片中盐酸水苏碱含量的方法，依次包括下述步骤：
1)取本品10片，除去包衣，精密称定，研细，取约2g，精密称定，置锥形瓶中，精密加入80％乙醇20ml，密塞，称定重量，超声提取30min，放冷，再称定重量，用80％乙醇补足减失的重量，摇匀，以1ml/min流速通过分别以3ml乙醇和3ml水活化的C18固相萃取小柱，用5ml水淋洗，弃去，再用5ml乙醇洗脱收集洗脱液，洗脱液于40℃下氮吹至近干，精密加入1ml乙醇溶解，用0.22μm有机滤膜过滤，取续滤液，即得供试品溶液；
2)取按处方比例及工艺制备的缺益母草阴性样品，按供试品溶液的制备方法制备阴性对照溶液；
3)精密称定盐酸水苏碱对照品17.42mg，至25ml量瓶中，加甲醇稀释至每1ml含盐酸水苏碱0.6940mg的溶液，精密吸取5ml，加甲醇稀释至25ml，得每1ml含盐酸水苏碱0.1388mg的对照品溶液；
4)分别称取供试品溶液、对照品溶液和阴性对照溶液，上Agilent1295-6550C三重四级杆液相质谱联用仪检测。
进一步的，上述的一种液质串联检测妇康宁片中盐酸水苏碱含量的方法，所述的液相色谱与质谱条件如下：
色谱柱：Agilent ZORBAX Eclipse Plus柱2.1×50mm，1.8m；流动相A为0.1％甲酸，流动相B为乙腈，采用梯度洗脱程序如下：0-2.0min，A、2-98％，B、98-2％；2.0-9.5min，A、5％，B、95％；9.5.-15min，A、70％，B、30％；流速0.8ml/min；柱温35℃；进样量2μl；电喷雾源ESI，正离子方式，选择多反应监测MRM，载气温度：150℃，载气流量：15L/min，雾化器压力40psi，鞘气温度350℃，鞘气流量：10L/min，毛细管电压3500V，定性定量离子：母离子m/z＝247.2，子离子m/z233.8和m/z205.2，碰撞能量分别为5V和20V，Frag均为380V。
与现有技术相比，本发明提供的采用液质串联检测妇康宁片中盐酸水苏碱含量的方法，检测快速，检测结果与采用药典检测的结果基本一致，为完善妇康宁片质量标准，控制其内在质量提供了一定的理论依据。
具体实施方式
下面结合具体实施方式，对本发明的权利要求做进一步的详细说明，但不构成对本发明的任何限制，任何在本发明权利要求保护范围所做的有限次的修改，仍在本发明的权利要求保护范围之内。
本发明所涉及的到百分含量浓度，除特殊说明外，溶质为液体的均为体积浓度，溶质为固体的均为质量浓度。
实施例1
1)取本品10片，除去包衣，精密称定，研细，取约2g，精密称定，置锥形瓶中，精密加入80％乙醇20ml，密塞，称定重量，超声提取30min，放冷，再称定重量，用80％乙醇补足减失的重量，摇匀，以1ml/min流速通过分别以3ml乙醇和3ml水活化的C18固相萃取小柱，用5ml水淋洗，弃去，再用5ml乙醇洗脱收集洗脱液，洗脱液于40℃下氮吹至近干，精密加入1ml乙醇溶解，用0.22μm有机滤膜过滤，取续滤液，即得供试品溶液；
2)取按处方比例及工艺制备的缺益母草阴性样品，按供试品溶液的制备方法制备阴性对照溶液；
3)精密称定盐酸水苏碱对照品17.42mg，至25ml量瓶中，加甲醇稀释至每1ml含盐酸水苏碱0.6940mg的溶液，精密吸取5ml，加甲醇稀释至25ml，得每1ml含盐酸水苏碱0.1388mg的对照品溶液；
4)分别称取供试品溶液、对照品溶液和阴性对照溶液，上Agilent1295-6550C三重四级杆液相质谱联用仪检测。
所述的液相色谱与质谱条件如下：
色谱柱：Agilent ZORBAX Eclipse Plus柱2.1×50mm，1.8m；流动相A为0.1％甲酸，流动相B为乙腈，采用梯度洗脱程序如下：0-2.0min，A、2-98％，B、98-2％；2.0-9.5min，A、5％，B、95％；9.5.-15min，A、70％，B、30％；流速0.8ml/min；柱温35℃；进样量2μl；电喷雾源ESI，正离子方式，选择多反应监测MRM，载气温度：150℃，载气流量：15L/min，雾化器压力40psi，鞘气温度350℃，鞘气流量：10L/min，毛细管电压3500V，定性定量离子：母离子m/z＝247.2，子离子m/z233.8和m/z205.2，碰撞能量分别为5V和20V，Frag均为380V。
阴性干扰试验：取对照品溶液、供试品溶液，阴性对照品溶液，按上述色谱条件测定。结果阴性对照品溶液色谱图中，在盐酸水苏碱色谱峰相应位置无干扰，表明本品中其他成分对盐酸水苏碱的测定无干扰
精密称取已知含量的同一批号样品6份，分别精密加入0.6940mg/ml的盐酸水苏碱对照品溶液0.7、1.0、1.3ml各2份，其余操作按下供试品溶液的制备方法，测定，计算，结果平均加样回收率为100.36％，RSD＝0.95％(n＝6)，表明本方法准确度较好
取四批样品，分别按上述含量测定方法测定，其检测结果基本一致，具体如下表所示：
序号 本法检测结果(mg/片) 药典检测结果(mg/片)
1 0.196 0.198
2 0.198 0.197
3 0.197 0.199
4 0.204 0.201

Claims (2)

1.一种液质串联检测妇康宁片中盐酸水苏碱含量的方法，其特征在于，依次包括下述步骤：
1)取本品10片，除去包衣，精密称定，研细，取约2g，精密称定，置锥形瓶中，精密加入80％乙醇20ml，密塞，称定重量，超声提取30min，放冷，再称定重量，用80％乙醇补足减失的重量，摇匀，以1ml/min流速通过分别以3ml乙醇和3ml水活化的C18固相萃取小柱，用5ml水淋洗，弃去，再用5ml乙醇洗脱收集洗脱液，洗脱液于40℃下氮吹至近干，精密加入1ml乙醇溶解，用0.22μm有机滤膜过滤，取续滤液，即得供试品溶液；
2)取按处方比例及工艺制备的缺益母草阴性样品，按供试品溶液的制备方法制备阴性对照溶液；
3)精密称定盐酸水苏碱对照品17.42mg，至25ml量瓶中，加甲醇稀释至每1ml含盐酸水苏碱0.6940mg的溶液，精密吸取5ml，加甲醇稀释至25ml，得每1ml含盐酸水苏碱0.1388mg的对照品溶液；
4)分别称取供试品溶液、对照品溶液和阴性对照溶液，上Agilent1295-6550C三重四级杆液相质谱联用仪检测。
2.根据权利要求1所述的一种液质串联检测妇康宁片中盐酸水苏碱含量的方法，其特征在于，所述的液相色谱与质谱条件如下：
色谱柱：Agilent ZORBAX Eclipse Plus柱2.1×50mm，1.8m；流动相A为0.1％甲酸，流动相B为乙腈，采用梯度洗脱程序如下：0-2.0min，A、2-98％，B、98-2％；2.0-9.5min，A、5％，B、95％；9.5.-15min，A、70％，B、30％；流速0.8ml/min；柱温35℃；进样量2μl；电喷雾源ESI，正离子方式，选择多反应监测MRM，载气温度：150℃，载气流量：15L/min，雾化器压力40psi，鞘气温度350℃，鞘气流量：10L/min，毛细管电压3500V，定性定量离子：母离子m/z＝247.2，子离子m/z233.8和m/z205.2，碰撞能量分别为5V和20V，Frag均为380V。
CN201610259400.3A 2016-04-25 2016-04-25 液质串联检测妇康宁片中盐酸水苏碱含量的方法 Pending CN105911187A (zh)

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CN117214337A (zh) * 2023-09-21 2023-12-12 甘肃广药白云山中药科技有限公司 一种检测药材成分的方法及其应用

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Application publication date: 20160831