同位素内标超高效液相色谱-串联质谱法测定膨化食品中丙烯酰胺  

Determination of acrylamide residue in puffed food by isotope dilution-ultra-high chromatography-tandem mass spectrometry

作　　者：罗佳 吴春霞[1,2] 周晓龙 LUO Jia;WU Chun-xia;ZHOU Xiao-long(Suzhou Municipul Center for Disrase Controd and Prerentiom,Sushou,Jiangst 215000,China)

机构地区：[1]苏州市疾病预防控制中心,江苏苏州215000 [2]江苏省食品安全风险监测重点实验室,江苏苏州215000

出　　处：《中国卫生检验杂志》2022年第14期1695-1698,共4页Chinese Journal of Health Laboratory Technology

基　　金：苏州市科技计划项目(医疗卫生应用基础研究)(SKJYD2021141)。

摘　　要：目的建立超高效液相色谱-串联质谱方法(UPLC-ESI-MS/MS),并对膨化食品中的丙烯酰胺进行定量分析。方法样品经超纯水提取,用Oasis HLB和Bond ElutAccucat固相萃取小柱净化。采用Atlantis dC18柱(2.1 mm×150 mm,3μm),以0.1%甲酸和乙腈为流动相进行梯度洗脱,电喷雾正离子模式电离,多反应监测模式检测,内标法定量,考察和优化样品前处理方法、色谱条件、质谱参数等,验证回收率、精密度等,以建立理想的检测方法。结果丙烯酰胺的质量浓度在1.0 ng/ml~1000.0 ng/ml与峰面积呈良好的线性,相关系数为0.999。方法定量限(S/N>10)为5μg/kg。在20μg/kg、100μg/kg、200μg/kg的添加水平下加标回收率为93.5%~105.0%,相对标准偏差为1.5%~6.3%。结论该方法具有快速、准确度和灵敏度高、重现性好,适用于膨化食品中痕量、超痕量丙烯酰胺的检测。Objective A ultra-high performance liquid chromatography-electrospray tandem quadrupole mass spectrometry(UPLC-ESI-MS/MS)method was developed for the quantitative analysis of acrylamide in puffed food.Methods Acrylamide in puffed food was extracted with ultrapure water and purified by SPE with Oasis HLB carteidge and Bond ElutAccuact cartridge.The liquid chromatography separation was performed on Atlantis dC18chromatographic column(2.1 mm×150 mm,3μm).0.1%formic acid and acetonitrile were used as mobile phases for gradient elution,electrospray ionization in positive ion mode,multi-reaction monitoring mode detection,quantification by internal standard method,sample pretreatment method,chromatographic conditions,mass spectrometry parameters were investigated and optimized to verify the recovery and precision,so as to establish an ideal detection method.Results Acrylamide had good linear relationship in the range of 1.0 ng/ml-1000.0 ng/ml,and the correlation coefficient was 0.999.The limit of quantitative(S/N>10)was 5μg/kg.Recovery of acrylamide from puffed food sample was evaluated at concentrations of 20μg/kg,100μg/kg and 200μg/kg.The recoveries of acrylamide were between 93.5%-105.0%with relative standard derivations within 1.5%-6.3%.Conclusion The rapid,accurate and sensitive UPLC-MS/MS method can be applied to monitor trace or ultra-trace acrylamide in puffed food.

关 键 词：超高效液相色谱-串联质谱法 丙烯酰胺 多反应监测 膨化食品 

分 类 号：O657[理学—分析化学]