溴衍生-固相萃取-UPLC-MS/MS法检测饼干中的丙烯酰胺  

Determination of acrylamide in biscuits by bromine derivatization-solid phase extraction coupled with ultra performance liquid chromatography-tandem mass spectrometry

作　　者：谢爱萍[1] 张学[1] 彭立核[1] 李佳伟[1] 王军淋[2] 吴平谷[2] XIE Ai-ping;ZHANG Xue;PENG Li-he;LI Jia-wei;WANG Jun-lin;WU Ping-gu(Jiashan County Center for Disease Control and Prevention,Zhejiang 314100,China;不详)

机构地区：[1]嘉善县疾病预防控制中心,浙江314100 [2]浙江省疾病预防控制中心

出　　处：《中国卫生检验杂志》2023年第10期1176-1179,共4页Chinese Journal of Health Laboratory Technology

摘　　要：目的建立饼干中的丙烯酰胺的溴衍生-固相萃取-超高效液相色谱-串联质谱测定法。方法样品中加入^(13)C_(3)-丙烯酰胺内标,用纯水提取,二氯甲烷除脂,取上清液加入溴化钾溶液、硫酸溶液和溴酸钾溶液混匀后,避光衍生。衍生物经HLB固相萃取柱富集,40%甲醇水淋洗除杂,乙酸乙酯洗脱,洗脱液氮吹至近干,流动相复溶。以0.1%甲酸水溶液-甲醇为流动相,经ACQUITY UPLC^(TM)BEH C_(18)(100 mm×2.1 mm,1.7μm)柱梯度分离。电喷雾正离子模式电离,多反应模式测定(MRM),内标法定量。结果丙烯酰胺衍生物(2,3-二溴丙酰胺)在5.0 ng/ml~500 ng/ml内,线性相关系数大于0.999;方法检出限为1.2μg/kg,定量限为4.0μg/kg;对饼干样本进行加标回收实验,在40μg/kg、200μg/kg、400μg/kg添加水平下加标回收率为91.63%~102.30%,相对标准偏差(RSD)在2.39%~3.38%(n=6)。结论本方法操作简单、快速、灵敏度高、选择性好,适用于饼干中丙烯酰胺的大批量检测。Objective A method was established for the determination of acrylamide in biscuits by bromine derivatization-solid phase extraction(SPE)-ultra performance liquid chromatography-tandem mass spectrometry(UPLC/MS/MS).Methods Acrylamide in the samples with ^(13)C_(3)-acrylamide as internal control was extracted with pure water,and then the fat in the solution was eliminated with dichloromethane.The supernatant was added with the solution of potassium bromide,sulfuric acid and potassium bromate,mixed up and placed in dark for derivation.The solution was loading on an HLB solid phase extraction(SPE)column for concentration,40%methanol aqueous was used for purification and ethyl acetate was used for elution;after blowing to near dry at a stream nitrogen,the drug residues were reconstituted with mobile phase and separated on an ACQUITY UPLC^(TM)BEH C_(18)(100 mm×2.1 mm,1.7μm)with 0.1%formic acid and methanol as mobile phase.The detection was accomplished on a triple quadrupole mass spectrometer with positive electrospray ionization in multiple reaction monitoring modes(MRM),and quantified by internal standard methods.Results The linear correlation coefficient(r)of acrylamide derivatives(2,3-dibromopropanamide)was greater than 0.999 in the range of 1.0 ng/ml to 1000 ng/ml.The limit of detection was 1.2μg/kg,and the limit of quantification was 4μg/kg.The recoveries were in the range of 91.63%-102.30%,and the relative standard deviations(RSDs)ranged from 2.39%to 3.38%(n=6),when acrylamide was spiked with 40μg/kg,200μg/kg,and 400μg/kg.Conclusion The method is rapid and simple,sensitive,and selective,which is suitable for batches determination of acrylamide in biscuits.

关 键 词：超高效液相色谱-串联质谱法 饼干 丙烯酰胺 

分 类 号：O657[理学—分析化学]