固相萃取-同位素内标-GC-MS/MS法测定根及根茎类中药材中18个多环芳烃残留量  

Determination of 18 polycyclic aromatic hydrocarbons in root and rhizome herbs by SPE-isotope dilution GC-MS/MS

作　　者：刘丽娜[1] 金红宇[1] 昝珂[1] 马双成[1] LIU Li-na;JIN Hong-yu;ZAN Ke;MA Shuang-cheng(National Institutes for Food and Drug Control,Beijing 102629,China)

机构地区：[1]中国食品药品检定研究院,北京102629

出　　处：《药物分析杂志》2023年第3期448-456,共9页Chinese Journal of Pharmaceutical Analysis

摘　　要：目的:建立了固相萃取-同位素内标-GC-MS/MS法测定根及根茎类中药材中18个多环芳烃的残留量,为评价根及根茎类中药材安全性提供有效分析手段。方法:采用氘代多环芳烃同位素内标,药材以乙腈提取,经C18固相萃取小柱净化后,采用GC-MS/MS测定,色谱柱为DM-17ms(30 m×0.25 mm, 0.25μm),程序升温,以多反应检测模式进行检测。结果:18个典型多环芳烃在2~50 ng·mL^(-1)内线性关系良好;在2~50μg·kg^(-1)内的平均回收率为63.8%~118.0%,RSD为0.45%~19.0%(n=3);方法定量限为0.5~1μg·kg^(-1)。结论:本方法操作简便,专属性强,灵敏度高,可满足根及根茎类中药材中18个典型多环芳烃残留的定量检测工作。Objective:To develop a SPE-isotope dilution GC-MS/MS method for the determination of the resi-dues of 18 polycyclic aromatic hydrocarbons(PAHs)in root and rhizome herbs.Methods:Using isotope as inter-nal standard,the sample was extracted by acetonitrile and purified by solid phase extraction on C18 cartridges.GC-MS/MS method was used for the assay.The chromatographic column was DB-17ms(30 m×0.25 mm,0.25μm)with temperature programming and MRM detection.Results:The calibration curves for the 18 kinds of typical PAHs were linear in the range of 2-50 ng·mL^(-1).The average recovery rate was in the range of 63.8%-118.0%,with RSD 0.45%-19.0%(n=3).The LOQs were 0.5-1μg·kg^(-1).Conclusion:This method is specific,sensitive,and can be used for residue detection of 18 typical kinds of PAHs in root and rhizome herbs.

关 键 词：多环芳烃 根及根茎类 中药材 同位素内标 气相色谱-三重四极杆串联质谱法 固相萃取 

分 类 号：R917[医药卫生—药物分析学]