摘要
基于改良的QuEChERS方法,建立同时测定果蔬中高氯酸盐、氯酸盐和溴酸盐的超高效液相色谱-串联质谱(ultra-high performance liquid chromatography-tandem mass spectrometry,UPLC-MS/MS)检测方法。实验以回收率为考察指标对N-丙基乙二胺、石墨化碳黑(graphitizing of carbon black,GCB)和C18三种吸附净化剂用量进行优化。样品经50%乙腈溶液提取2次,提取液经GCB 40 mg和C18200 mg混合吸附剂萃取净化,经IC-PakTM Anion HR色谱柱分离,UPLC-MS/MS进行检测,基质外标法进行定量分析。3种基质中(苹果、梨和青菜)高氯酸盐、氯酸盐和溴酸盐在0.5~100 mg/L范围内线性关系良好,线性相关系数均大于0.99。在5.0、20.0 mg/kg和50.0 mg/kg三个添加水平下的平均回收率为80.3%~110.1%,相对标准偏差在2.1%~9.6%之间,方法检出限为0.5~1.5 mg/kg,方法定量限为2.0~5.0 mg/kg。该方法快速便捷、灵敏可靠、回收率稳定,适用于果蔬中高氯酸盐、氯酸盐和溴酸盐的同时测定。
A modified quick,easy,cheap,effective,rugged and safe(QuEChERS)method coupled with ultra-high performance liquid chromatography-tandem mass spectrometry(UPLC-MS/MS)was developed for the determination of perchlorate,chlorate and bromate in vegetables and fruits.The type and amount of sorbents including primary secondary amine(PSA),graphitized carbon black(GCB)and C18,were optimized based on the recoveries.Samples were extracted twice with 50%acetonitrile/water.The extract was purified with a mixture of 40 mg of GCB and 200 mg of C18,separated on an IC-PakTM Anion HR column,and detected by UPLC-MS/MS.The matrix-matched external standard method was used for quantitation.Good linearity was achieved for the analytes in the concentration range of 0.5–100 mg/L with correlation coefficients all greater than 0.99.The average recoveries for all the compounds at spiked concentration levels of 5.0,20.0 and 50.0μg/kg ranged from 80.3%to 110.1%,with relative standard deviations(RSDs)from 2.1%to 9.6%.The limits of detection(LODs)and the limits of quantification(LOQs)were 0.5–1.5 mg/kg and 2.0–5.0 mg/kg,respectively.The developed method proved to be rapid,convenient,sensitive,accurate,stable,and suitable for simultaneous determination of perchlorate,chlorate and bromate in vegetables and fruits.
作者
盛华栋
潘项捷
张水锋
刘敏芳
施元旭
王璐璐
陆文琪
SHENG Huadong;PAN Xiangjie;ZHANG Shuifeng;LIU Minfang;SHI Yuanxu;WANG Lulu;LU Wenqi(Zhejiang Fangyuan Checking Group Co.Ltd.,Hangzhou 310018,China)
出处
《食品科学》
EI
CAS
CSCD
北大核心
2020年第10期324-329,共6页
Food Science
基金
浙江省质量技术监督局科研计划项目(20180116)
浙江省质量技术监督局科研计划项目(20180344)。
