改进的QuEChERS/超高效液相色谱-串联质谱法测定蜂蜜中的丙烯酰胺  

Determination of Acrylamide in Honey Samples by Modified QuECh⁃ERS/Ultra High Performance Liquid Chromatography-Tandem Mass Spectrometry

作　　者：张琳昀[1] 吉文亮[1] 沈菲 王鑫楠 钟诚 朱峰[1] ZHANG Lin-yun;JI Wen-iang;SHEN Fei;WANG Xin-nan;ZHONG Cheng;ZHU Feng(Jiangsu Provincial Center for Disease Prevention and Control,Nanjing 210009,China;Waters Corporation,Shanghai 200120,China)

机构地区：[1]江苏省疾病预防控制中心,江苏南京210009 [2]沃特世科技(上海)有限公司,上海200120

出　　处：《分析测试学报》2023年第10期1272-1278,共7页Journal of Instrumental Analysis

基　　金：食品中丙烯酰胺的测定(GB 5009.204-2014)修订项目(spaq-2022-22);江苏省重点研发计划(社会发展)项目(BE2021740);江苏省卫生健康委员会医学科研项目(M2021028)。

摘　　要：基于改进的基质分散固相萃取(QuEChERS)法,建立了超高效液相色谱-串联质谱检测蜂蜜中丙烯酰胺的方法。蜂蜜样品经纯水溶解分散后,加入乙腈提取,采用QuEChERS法净化。以0.1%甲酸水溶液和甲醇为流动相梯度洗脱,丙烯酰胺经ZORBAX RRHD Eclipse Plus C_(18)色谱柱(3.0 mm×150 mm,1.8µm)分离,在电喷雾电离源(ESI)正离子模式下,采用多反应监测(MRM)模式进行检测,内标法定量。丙烯酰胺在2.0~500 ng/mL范围内线性关系良好,相关系数(r^(2))为0.9997,方法检出限(LOD)和定量下限(LOQ)分别为0.42µg/kg和1.38µg/kg。蜂蜜样品中,丙烯酰胺在低、中、高3个加标水平下的平均回收率为89.2%~96.3%,相对标准偏差(RSD,n=6)为2.2%~4.2%。采用建立的方法对30份市售蜂蜜进行测定,丙烯酰胺的检出率为100%,含量为2.5~40.4µg/kg。该方法简单、快速,灵敏度高、准确性好,适用于蜂蜜中丙烯酰胺的测定。An analytical method for the determination of acrylamide in honey samples by modified QuEChERS using ultra high performance liquid chromatography-tandem mass spectrometry was es-tablished.After dissolved by water,honey samples was extracted by acetonitrile,and then the ex-tracted supernatant was cleaned by matrix dispersion solid phase extraction.The target was separated by ZORBAX RRHD Eclipse Plus C_(18) column(3.0 mm×150 mm,1.8µm)using 0.1%formic acid solution and methanol as mobile phase by gradient elution,and analyzed in positive electrospray ion-ization mode by multiple reaction monitoring(MRM)mode.Acrylamide was quantified by internal standard method.The analyte showed a good relationship in concentration range of 2.0-500 ng/mL,with a correlation coefficient(r^(2))of 0.9997.The limits of detection and quantitation of the method was 0.42µg/kg and 1.38µg/kg,respectively.Average recoveries of acrylamide at low,medium and high spiked levels in honey matrices were 89.2%-96.3%,and relative standard deviations(RS-Ds,n=6)were 2.2%-4.2%.The proposed method was applied for the determination of acrylamide in 30 honey samples,and all samples showed positive results.The acrylamide contents of 30 honey samples ranged from 2.5 to 40.4µg/kg.This method was suitable for analysis of acrylamide in honey samples with the advantages of simplicity,rapidity,high sensitivity and accuracy.

关 键 词：QUECHERS 超高效液相色谱-串联质谱法 蜂蜜 丙烯酰胺 

分 类 号：O657.7[理学—分析化学] TS201.6[理学—化学]