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
周颖 1徐哲 2张文婷 1周越美 3徐潇颖 1赵维良 3潘英妮 2郑成1
作者信息
- 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. 沈阳药科大学,沈阳 110000
- 3. 杭州师范大学药学院,杭州 311121
- 折叠
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0～26 403 μg·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.
Abstract
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,1.7 μm)as the stationary phase,gradient elution was carried out with methanol-0.1％formic acid aqueous solution as the mobile phase,13C3 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 0-26 403 μg·kg-1.These contents exceeded the regulations stipulated by some nations or organi-zations,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 evalua-tion 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/QuEChERSKey words
acrylamide/8 famous medicines from Zhejiang/ultra high performance liquid chromatography-tandem mass spectrometry/content determination/risk assessment/QuEChERS引用本文复制引用
基金项目
浙江省药品监督管理局科技计划项目(2019010)
出版年
2024
NETL
NSTL
万方数据