分散固相萃取-超高效液相色谱-三重四级杆液质法测定中药材中展青霉素

Determination of patulin in Chinese herbs by UHPLC- triple quadrupole MS with dispersive solid phase extraction

目的建立中药材中展青霉素的超高效液相色谱-三重四级杆液质法(UHPLC-MS/MS)测定方法。方法样品经果胶酶酶解,用乙腈水提取,提取液依次通过无水硫酸镁-无水醋酸钠(4∶1)混合粉末进行分散固相萃取和多功能净化柱净化去除杂质,用高效液相色谱-三重四级杆串联质谱进行分析测定。结果展青霉素在5 ng/ml^250 ng/ml范围内与离子流峰面积呈良好的线性关系,线形方程为Y=5.37×103X+151,r=0.9998,回收率在71%~99%之间。药材中检测限为0.3μg/kg^0.5μg/kg。结论本法灵敏、快速、准确、专属性强,可用于中药中展青霉素的测定。

Objective To establish a UHPLC - MS/MS method for determination of patulin in Chinese herbs. Methods After pectinase enzymolysis and extraction by acetonitrile water solution, the sample extraction solution were conducted dispersive sol- id phase extraction by mix powder of MgSO4 and NaAC （4：1 ）, then purified on Mycrosep228 AlaPat column, finally analyzed by UHPLC - triple quadrupole MS. Results Patulin showed good linear relationship with ion current peak area within the range of 5 ng/ml- 250 ng/ml, and the linear equation was Y = 5.37× 103 X ＋ 151, r = 0. 9998. The recovery was between 71% - 99%. The LODs in herbs were in the range of 0.3 μg/kg - 0.5 μg/kg. Conclusion The method is sensitive, rapid, accurate and specific enough to determine patulin in Chinese herbs.