分散固相萃取-高效液相色谱-串联质谱法同时测定保健品片剂中5种黄芩素类化合物

Simultaneous determination of five baicaleins in healthy product tablets by dispersive solid-phase extraction-high performance liquid chromatography-tandem mass spectrometry

基于分散固相萃取-高效液相色谱-串联质谱技术(DSPE-HPLC-MS/MS),建立了同时测定保健品片剂中野黄芩素、4′-羟基汉黄芩素、去甲汉黄芩素、黄芩素和汉黄芩素的分析方法。以10 mL丙酮提取保健品片剂中的目标成分,75 mg C18吸附剂进行净化。通过优化提取溶剂、吸附剂的种类和用量,达到了提取和净化的目的。结果表明,5种目标物在各自的线性范围内具有良好的线性关系,相关系数(r)均大于0.99,检出限为0.5~40μg/kg,定量限为2.0~120μg/kg。使用3种保健品片剂基质进行定量限的1倍、5倍、10倍3个添加水平的加标回收试验,5个目标物的平均回收率为83.1%~106.5%,精密度为0.97%~4.52%。该方法操作简单、灵敏度高、重现性好,适用于保健品片剂中黄芩素类化合物的同时测定。

A method based on dispersive solid-phase extraction-high performance liquid chromatography-tandem mass spectrometry(DSPE-HPLC-MS/MS)was developed for the simultaneous determination of five analytesscutellarein,4′-hydroxywogonin,norwogonin,baicalein,and wogoninin healthy product tablets.The samples were extracted with 10 mL acetone and purified on 75 mg C18.The types and dosages of the extracted solvents and adsorbents were optimized.The results showed that these five analytes exhibited good linear relationships in their respective linear ranges.The correlation coefficients(r)were more than 0.99.The detection limits and quantitative limits were 0.5-40μg/kg and 2.0-120μg/kg,respectively.Recovery tests were carried out using three kinds of health product tablet matrices.The concentrations were one,five,and ten times the quantitative limit.The average recovery of these five targets was 83.1%to 106.5%,with relative standard deviations(RSDs)ranging from 0.97%to 4.52%.This method is easy to operate,and it shows high sensitivity and good reproducibility.Thus,it is suitable for the simultaneous determination of the target compounds in health tablets.