摘要
目的:建立一种快速测定黑木耳中米酵菌酸残留量检测的QuEChERS-UHPLC-MS/MS方法。方法:利用加标样品对提取溶剂、提取时间、吸附剂种类及吸附剂用量等参数进行优化,样品用1%氨水—甲醇提取,经C;吸附剂净化,采用电喷雾电离源负离子多反应监测模式分析,外标法定量。结果:样品在4 min内完成分析,米酵菌酸在质量浓度0.50~10.00 ng/mL内线性关系良好,相关系数(r)为0.9983,检出限(LOD)为2μg/kg。在空白样品中添加低、中、高3个浓度水平的日内平均回收率为74.4%~91.6%(n=6),日间平均回收率为74.9%~89.4%(n=3),相对标准偏差(RSD)为3.3%~9.2%。结论:该方法操作简单、快速、回收率优良,重复性好、检测限低于现有检测标准要求,可用于黑木耳中米酵菌酸含量的定性和定量分析。
Objective:A rapid method for determination of bongkrekic acid in Auricularia auricular was developed using QuEChERS in combination with UHPLC-MS/MS.Methods:In this study,Several important experimental parameters,including type of extraction solvent,extraction time,adsorbent type and adsorbent dosage were effectively optimized using spiked samples.The sample were shaken with methanol containing 1%ammonia water,and then carried out by the C;adsorbent purification.Results:The bongkrekic acid was determined within 4 minutes by negative ion multiple reaction monitoring mode analysis and external standard method.The linear range was 0.05~10.00 ng/mL(r>0.9983).The limit of detection(LOD)was 2μg/kg,respectively.The average recovery rate at different levels(low,medium and high)the intra-batch(n=6)was 74.4%~91.6%,the inter-batch(n=3)were 74.9%~89.4%with a RSD ranging from 3.3%~9.2%.Conclusion:The developed method shows simple,rapid,excellent recovery and stable repeatability,and the limit of detection lower than the existing detection standards.It is suitable for the effective detection of bongkrekic acid in Auricularia auricular samples.
作者
黄永桥
马凯
吴新文
高亮
简银池
路瑶
杨昌彪
HUANG Yong-qiao;MA Kai;WU Xin-wen;GAO Liang;JIAN Yin-chi;LU Yao;YANG Chang-biao(Guizhou Testing Technology Research and Application Center,Guiyang,Guizhou 550014,China;Guizhou Academy of Testing and Analysis,Guiyang,Guizhou 550014,China)
出处
《食品与机械》
北大核心
2022年第7期63-67,共5页
Food and Machinery
基金
国家重点研发计划(编号:2017YFC1601800)
贵州省科技计划项目(编号:黔科合服企[2019]4001,黔科中引地[2021]4026)
DNA条形码食品安全检测平台项目(编号:GXYF-2018-002)。
