高温炮制后白术中丙烯酰胺和天冬酰胺的多壁碳纳米管分散固相萃取和液相色谱串联质谱同时测定法  

Simultaneous determination of acrylamide and L-asparagine in Atractylodis macrocephalae rhizoma after thermal processing by multi-walled carbon nanotubes-dispersive solid-phase extraction combined with liquid chromatography-tandem mass spectrometry

作　　者：徐潇颖 梁晶晶 朱炳祺 郎雯君 刘柱 XU Xiao-ying;LIANG Jing-jing;ZHU Bing-qi;LANG Wen-jun;LIU Zhu(National Key Laboratory of Market Supervision(Quality and Safety of Functional Food),Food InspectionInstituteof Zhejiang Institute for Food and Drug Control,Hangzhou Zhejiang,310000,China;College of medical technology and Information Engineering,Zhejiang Chinese Medical University,Hangzhou Zhejiang,310000,China)

机构地区：[1]国家市场监管重点实验室(功能食品质量与安全)浙江省食品药品检验研究院食品检验研究所,浙江杭州310000 [2]浙江中医药大学医学技术与信息工程学院,浙江杭州310000

出　　处：《职业与健康》2023年第10期1306-1311,共6页Occupation and Health

基　　金：浙江省药品监督监管系统科研项目(2022015);浙江中医药科技计划科研项目(2021ZQ024);浙江教育厅科研项目(Y202045160)。

摘　　要：目的建立一种同时测定白术中丙烯酰胺和天冬酰胺的方法,分析白术高温炮制过程中丙烯酰胺和天冬酰胺的变化规律,为炮制工艺研究提供参考依据。方法通过多壁碳纳米管分散固相萃取和液相色谱串联质谱技术实现白术中天冬酰胺和丙烯酰胺的同时测定。利用该方法,在控制不同炮制温度和炮制时间条件下,分别测定白术高温炮制样品中天冬酰胺和丙烯酰胺含量。通过暴露限值(margin of exposure,MOE)对白术中丙烯酰胺污染进行风险评估。结果最终优化的丙烯酰胺和天冬酰胺同时测定方法下,获得的天冬酰胺回收率为98.4%~103.2%,相对标准偏差(theretaationstandarddeviation,RSD)为2.5%~3.6%;丙烯酰胺的回收率在97.5%~101.9%,RSD为1.9%~3.1%。丙烯酰胺在1~50 ng/mL,天冬酰胺在25~1000 ng/mL线性关系良好,相关系数均≥0.99,丙烯酰胺的检出限为0.003 mg/kg,天冬酰胺的检出限为0.1 mg/kg。白术炮制过程中,天冬酰胺随时间增加呈下降趋势,丙烯酰胺含量随炮制时间先增加后下降。根据炮制后白术中丙烯酰胺含量变化最低值79.3μg/kg和最高值1558.9μg/kg,得到最低MOE值673.6,表明存在一定的安全风险。结论本研究建立并验证了丙烯酰胺和天冬酰胺同时测定的方法,白术经过炮制以后丙烯酰胺浓度显著升高,导致一定的安全风险隐患,需要综合考虑以进一步完善和规范化炮制工艺。Objective To establish a method for simultaneous determination of acrylamide andL-asparagine in Atractylodis macrocephalae rhizome(AMR),analyze the content change of acrylamide and L-asparagine during the thermal processing of AMR,so as to providebasis for the research of processing technology.Methods The simultaneous determination of L-asparagine and acrylamide in AMR was realized by dispersed solid phase extraction using multi-walled carbon nanotubes(MWCNTs)and liquid chromatography tandem mass spectrometry(LC-MS/MS).Using this method,the contents of L-asparagine andacrylamide in processed AMR samples were determined under different processing temperature and time.The risk of acrylamide contamination in AMR was evaluated by margin of exposure(MOE).Results In the validation of the optimized method,the recoveries of L-asparagine were 98.4%-103.2%with relative standard deviation(RSD)of 2.5%-3.6%.The recoveries of acrylamide were 97.5%-101.9%with RSD of 1.9%-3.1%.The linear relationships of acrylamide and L-asparagine were good within the range of 1-50 ng/mL and 25-1000 ng/mL respectively,and the correlation coefficients were≥0.99.The detection limit of acrylamide and L-asparagine was 0.003 mg/kg and 0.1 mg/kg respectively.During the processing of AMR,L-asparagine showed a downward trend with the increase of time,and the content of acrylamide first increased and then decreased with the processing time.According to the change of acrylamide content in AMR after processing,the lowest value was 79.3μg/kg and the highest value was 1558.9μg/kg,which led to the lowest MOE value of 673.6,indicating safety risk.Conclusions The study establishes and verifies a method for the simultaneous determination of acrylamide and L-asparagine.After the thermal processing of AMR,the concentration of acrylamide increases significantly,resulting in potential safety risks.Comprehensive consideration was needed to further improve and standardize the processing technology.

关 键 词：丙烯酰胺 天冬酰胺 白术 高温炮制 暴露限值 

分 类 号：R115[医药卫生—公共卫生与预防医学]