摘要
目的建立一种QuEChERS前处理净化结合超高效液相色谱-串联质谱法(ultra performance liquid chromatography-tandem mass spectrometry,UPLC-MS/MS)快速检测汉中面皮中米酵菌酸含量的方法。方法面皮样品采用乙腈-水(8:2,V:V)超声提取,QuEChERS净化处理,浓缩、定容,选用Thermo(100 mm×2.1 mm,1.8μm)色谱柱分离,以乙腈和0.1%甲酸水溶液进行梯度洗脱,电喷雾离子源(electron spray ionization,ESI),负离子多反应监测(multiple reaction monitoring,MRM)模式,以标准曲线法定量。结果米酵菌酸在1~100 ng/mL范围内线性关系良好,相关系数(r^(2))大于0.999,在2、10、50μg/kg低中高3个加标水平下,加标回收率为86.7%~90.0%,相对标准偏差(relative standard deviation,RSD)为2.3%~2.9%,检出限为0.5μg/kg,定量限为1.5μg/kg。所有实际样品均未检出米酵菌酸。结论该方法前处理简单、分析快速、回收率高、灵敏度高,可为汉中面皮中米酵菌酸的质量控制提供参考。
Objective To establish a method for rapid determination of bongkrekic acid content in Hanzhong Mianpi by ultra performance liquid chromatography-tandem mass spectrometry(UPLC-MS/MS)combined with QuEChERS purification.Methods Hanzhong Mianpi samples were extracted by acetonitrile-water(8:2,V:V)ultrasonic extraction,purified by QuEChERS,concentrated,constant volume,separated by Thermo(100 mm×2.1 mm,1.8μm)chromatographic column,gradient eluted by acetonitrile and 0.1%formic acid aqueous solution,quantified by standard curve method with electric spray ion source(ESI),multiple reaction monitoring(MRM)mode.Results The linear relationship of bongkrekic acid was good within the range of 1-100 ng/mL,with a correlation coefficient(r^(2))greater than 0.999.At 3 spiked levels of 2,10 and 50μg/kg,the spiked recovery rate was 86.7%-90.0%,the relative standard deviation(RSD)was 2.3%-2.9%,the limit of detection was 0.5μg/kg,and the limit of quantitation was 1.5μg/kg.All actual samples did not detect any citric acid.Conclusion This method has simple pre-treatment,fast analysis,high recovery rate,and high sensitivity,which can provide reference for the quality control of bongkrekic acid in Hanzhong Mianpi.
作者
卢军
黄文
李崇勇
缑慧君
徐姗娜
LU Jun;HUANG Wen;LI Chong-Yong;GOU Hui-Jun;XU Shan-Na(Food and Drug Supervision Inspection and Testing Center of Hanzhong,Hanzhong 723000,China)
出处
《食品安全质量检测学报》
2025年第11期228-233,共6页
Journal of Food Safety and Quality
基金
陕西省市场监督管理局2022年度科技计划项目(2022KY27)。
关键词
超高效液相色谱-串联质谱法
QuEChERS净化
米酵菌酸
汉中面皮
ultra performance liquid chromatography-tandem mass spectrometry
QuEChERS purification
bongkrekic acid
Hanzhong Mianpi
