同位素内标-UHPLC-MS/MS联用QuEChERS法检测“浙八味”等道地药材中丙烯酰胺含量及初步风险评估  

Determination and preliminary risk assessment of acrylamide in“8 famous medicines from Zhejiang”by isotope-labeled internal standard-UHPLC-MS/MS in combination with QuEChERS method

作　　者：周颖 徐哲[3] 张文婷 周越美 徐潇颖 赵维良 潘英妮[3] 郑成 ZHOU Ying;XU Zhe;ZHANG Wen-ting;ZHOU Yue-mei;XU Xiao-ying;ZHAO Wei-liang;PAN Ying-ni;ZHENG Cheng(Zhejiang Institute for Food and Drug Control,NMPA Key Laboratory of Quality Evaluation of Traditional Chinese Medicine(Traditional Chinese Patent Medicine),Hangzhou 310052,China;Hangzhou Normal University,Hangzhou 311121,China;Shenyang Pharmaceutical University,Shenyang 110000,China)

机构地区：[1]浙江省食品药品检验研究院,国家药品监督管理局中成药质量评价重点实验室,杭州310052 [2]杭州师范大学药学院,杭州311121 [3]沈阳药科大学,沈阳110000

出　　处：《药物分析杂志》2024年第6期1017-1023,共7页Chinese Journal of Pharmaceutical Analysis

基　　金：“浙八味”“新浙八味”炮制品中丙烯酰胺(AM)残留检测研究-浙江省药品监督管理局科技计划项目(2019010)。

摘　　要：目的:以“浙八味”为对象,研究建立中药材中丙烯酰胺含量的通用测定方法,并根据测定结果进行初步风险评估。方法:样品经过优化的QuEChERS技术提取后,采用同位素内标-超高效液相色谱-串联质谱(UHPLC-MS/MS)法测定丙烯酰胺的含量,以Phenomenex Kinetex C18色谱柱(100 mm×2.1 mm, 1.7μm)为固定相,以甲醇-0.1%甲酸水溶液为流动相进行梯度洗脱,以13C3丙烯酰胺为内标,以多反应监测(MRM)模式进行检测丙烯酰胺的残留量。结果:247批样品中丙烯酰胺的含量范围为0~26 403μg·kg^(-1),含量超过部分国家或组织的规定,长期使用存在一定的安全风险。结论:本研究所建立的方法快速、简单,具有较好的灵敏度与重复性,为“浙八味”等道地中药材中丙烯酰胺的质量控制和安全性评价提供了科学依据。Objective:To determine the content of acrylamide in“8 famous medicines from Zhejiang”,and to carry out the preliminary risk assessment based on the determination results.Methods:After optimization of QuEChERS extraction,the content of acrylamide was determined by the method of isotope-labeled internal standard-ultra high performance liquid chromatography-tandem mass spectrometry(isotope-labeled IS-UHPLC-MS/MS).The determination was carried out with a Phenomenex Kinetex C18 column(100 mm×2.1 mm,1.7μm)as the stationary phase,gradient elution was carried out with methanol-0.1%formic acid aqueous solution as the mobile phase,13 C3 acrylamide as the internal standard,and multiple reaction monitoring(MRM)mode was used to detect the residual acrylamide.Results:The content ranges of acrylamide in 247 batches of samples were 0-26403μg·kg^(-1).These contents exceeded the regulations stipulated by some nations or organizations,and posed certain safety risks in long-term use.Conclusion:The method established in this study is rapid,simple,sensitive and reproducible,and will lay a scientific basis for the quality control and safety evaluation of acrylamide in“8 famous medicines from Zhejiang”and other genuine medicinal materials.

关 键 词：丙烯酰胺 浙八味 超高效液相色谱-串联质谱 含量测定 风险评估 QUECHERS 

分 类 号：R917[医药卫生—药物分析学]