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引用本文:刘东升,朱琳,苏蕊,徐继军,姚世霞,朱旭江.沉香化滞丸中松香酸的HPLC和UPLC-Q-TOF检测方法研究[J].中国现代应用药学,2020,37(14):1726-1729.
LIU Dongsheng,ZHU Lin,SU Rui,XU Jijun,YAO Shixia,ZHU Xujiang.Research on HPLC and UPLC-Q-TOF for the Determination of Abietic Acid in Chenxiang Huazhi Pills[J].Chin J Mod Appl Pharm(中国现代应用药学),2020,37(14):1726-1729.
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沉香化滞丸中松香酸的HPLC和UPLC-Q-TOF检测方法研究
刘东升1,2, 朱琳1,2, 苏蕊1,2, 徐继军1,2, 姚世霞1,2, 朱旭江1,2
1.甘肃省药品检验研究院, 兰州 730070;2.甘肃省中藏药检验检测技术工程实验室, 兰州 730070
摘要:
目的 建立沉香化滞丸中松香酸的HPLC和UPLC-Q-TOF检测方法。方法 采用HPLC测定沉香化滞丸中非法存在的松香酸,并对阳性结果采用UPLC-Q-TOF进行验证。结果 松香酸浓度在1.40~21.03 μg·mL-1与峰面积积分值呈良好的线性关系,仪器精密度RSD为0.2%,加样回收率为99.5%,RSD为1.7%。通过保留时间、最大吸收波长、母离子(m/z 303.23)及其子离子(m/z 285.22,257.22,149.13,123.11)4个方面的信息,确认13批沉香化滞丸中10批样品非法掺入了松香酸。结论 该方法操作简便、准确,快速,灵敏度高,适合对沉香化滞丸中非法添加松香酸的检测。对沉香化滞丸质量控制方面,建议增加对松香酸非法添加的检验项目。
关键词:  沉香化滞丸  松香酸  HPLC  UPLC-Q-TOF
DOI:10.13748/j.cnki.issn1007-7693.2020.14.011
分类号:R917.101
基金项目:甘肃省食品药品科研项目(2018GSFDA005,2018GSFDA037)
Research on HPLC and UPLC-Q-TOF for the Determination of Abietic Acid in Chenxiang Huazhi Pills
LIU Dongsheng1,2, ZHU Lin1,2, SU Rui1,2, XU Jijun1,2, YAO Shixia1,2, ZHU Xujiang1,2
1.Gansu Institute for Drug Control, Lanzhou 730070, China;2.Gansu Inspection and Testing Technical Engineering Laboratory for Chinese Hebal and Tibetan Midicine, Lanzhou 730070, China
Abstract:
OBJECTIVE To establish HPLC and UPLC-Q-TOF identification determination methods for abietic acid, an illegal additive in Chenxiang Huazhi pills. METHODS HPLC was used to determine the illicit presence of abietic acid in Chenxianghuazhi Pills. The positive results were verified by UPLC-Q-TOF. RESULTS The concentration of abietic acid in the range of 1.40-21.03 μg·mL-1 showed a good linear relationship with the peak area integral value. The precision RSD was 0.2%, the sample recovery rate was 99.5%, and the RSD was 1.7%. The obtained retention time of HPLC, the maximum absorption wavelength, mother ion (m/z 303.23), fragment ions (m/z 285.22, 257.22, 149.13, 123.11), the identification of abietic acid was performed in 13 batches Chenxiang Huazhi pills. It showed that 10 samples were added the substance containing abietic acid. CONCLUSION The method is simple, accurate, rapid, and sensitive, which is helpful for the detection of abietic acid in Chenxiang Huazhi pills. For the quality control of Chenxiang Huazhi Pills, it is recommended to add the inspection item for illegal addition of abietic acid.
Key words:  Chenxiang Huazhi pills  abietic acid  HPLC  UPLC-Q-TOF
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