沉香化滞丸中松香酸的HPLC和UPLC-Q-TOF检测方法研究

Research on HPLC and UPLC-Q-TOF for the Determination of Abietic Acid in Chenxiang Huazhi Pills

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1.40~21.03μg·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。

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 1.40-21.03μg·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.