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

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.