摘要
目的 建立测定龙胆泻肝丸中木通苯乙醇苷B含量的超高效液相色谱串联质谱法。方法 色谱柱为Waters ACQUITY UPLC®BEH C_(18)柱(100 mm×2.1 mm,1.7μm),流动相为乙腈-0.1%甲酸溶液(梯度洗脱),流速为1.0 mL/min,柱温为30℃,进样量为10μL。电喷雾离子源(ESI-),多反应监测模式(MRM),毛细管电压0.5 kV,锥孔电压-55 V,锥孔气流量50 L/h,脱溶剂气流量900 L/h,脱溶剂气温度550℃,木通苯乙醇苷B检测离子对m/z 477→161、m/z 477→133和m/z 477→315。结果 木通苯乙醇苷B质量浓度在0.103 4~5.170 0μg/mL范围内与峰面积线性关系良好(r=0.999 9);精密度、稳定性、重复性试验结果的RSD均小于4.0%;平均加样回收率为104.96%,RSD为4.36%(n=6)。36批样品中均含有木通苯乙醇苷B,含量为14.42~255.02μg/g。结论 所建方法精密度、稳定性、重复性均较好,可用于测定龙胆泻肝丸中木通苯乙醇苷B的含量,并可快速甄别是否有不投料或伪品假冒行为。
Objective To establish a method for the content determination of calceorioside B in Longdan Xiegan Pills by ultra-performance liquid chromatography-tandem mass spectrometry(UPLC-MS/MS).Methods The chromatographic column was Waters ACQUITY UPLC®BEH C_(18) column(100 mm×2.1 mm,1.7μm),the mobile phase was acetonitrile-0.1%formic acid solution with gradient elution,the flow rate was 1.0 mL/min,the column temperature was 30℃,and the injection volume was 10μL.Electric spray ion(ESI-)source was adopted with multi-reaction monitoring(MRM)mode,the capillary voltage was 0.5 kV,the cone hole voltage was-55 V,the cone hole gas flow was 50 L/h,the desolvent gas flow was 900 L/h,the desolvent gas temperature was 550℃,the ion pairs of calceorioside B were m/z 477→161,m/z 477→133 and m/z 477→315 were detected.Results The linear range of calceorioside B was 0.1034-5.1700μg/mL(r=0.9999).The RSDs of precision,stability and repeatability tests were less than 4.0%.The average recovery of calceorioside B was 104.96%with an RSD of 4.36%(n=6).The 36 batches of samples all contained calceorioside B,the content of which was in the range of 14.42-255.02μg/g.Conclusion The establiashed method has good precision,stability and repeatability,it can be used for the content determination of calceorioside B in Longdan Xiegan Pills,and can quickly identify whether there is no feeding or a counterfeit passing off as the real thing behavior.
作者
周云峰
邓杰华
黄招光
吴喆
黄炳泉
杨建冬
ZHOU Yunfeng;DENG Jiehua;HUANG Zhaoguang;WU Zhe;HUANG Bingquan;YANG Jiandong(The Inspection and Testing Center of Yichun,Yichun,Jiangxi,China 336000)
出处
《中国药业》
CAS
2022年第22期67-71,共5页
China Pharmaceuticals
基金
江西省药品监督管理局科研项目[2021KY24]。
