基于QuEChERS的超高效液相色谱-串联质谱法快速测定果蔬中双酚类物质  

Rapid Determination of Bisphenols in Fruits and Vegetables by QuEChERS-Ultra-High Performance Liquid Chromatography-Tandem Mass Spectrometry

作　　者：赵斌[1] 谭学蓉[1] 付瑜[1] 薛鸣[2] 许东海[1] 梁秀川 张丽 ZHAO Bin;TAN Xue-Rong;FU Yu;XUE Ming;XU Dong-Hai;LIANG Xiu-Chuan;ZHANG Li(Guangyuan Center for Disease Control and Prevention,Guangyuan 628000,China;Hangzhou Center for Disease Control and Prevention,Hangzhou 310006,China)

机构地区：[1]广元市疾病预防控制中心,广元628000 [2]杭州市疾病预防控制中心,杭州310006

出　　处：《分析化学》2022年第5期810-818,I0028-I0030,共12页Chinese Journal of Analytical Chemistry

基　　金：广元市科技计划项目(No.19ZDYF0016)资助。

摘　　要：建立了超高效液相色谱-三重四极杆串联质谱法(UPLC-MS/MS)同时测定水果(橙子、梨、猕猴桃、葡萄)和蔬菜(豇豆、韭菜、土豆、西蓝花)中8种双酚类物质(BPs)的分析方法。以QuEChERS处理技术为基础,选用乙腈为提取剂,NaAC为萃取盐,考察了基质效应(ME)和萃取回收率(RE)对过程效率(PE)的影响,选择33 mg N-丙基乙二胺(PSA)、33 mg石墨化碳黑(GCB)和10 mg C_(18)混合吸附剂为净化剂。以甲醇和0.1 mmol/L NH_(4)HCO_(3)溶液为流动相,采用Waters BEH C_(18)(100 mm×2.1 mm,1.7μm)色谱柱分离;采用电喷雾离子源,在负离子、多反应监测模式下,使用同位素内标法进行定量检测分析。结果表明,在8 min内,可完成8种BPs的色谱分离,在线性范围内线性关系良好,相关系数(R^(2))均大于0.9990,检出限(LOD)为0.01~0.10μg/kg,定量限(LOQ)为0.03~0.35μg/kg;在不同果蔬基质样品中,8种BPs的平均加标回收率为67.2%~117.8%,相对标准偏差(RSD)为0.1%~8.3%。采用本方法检测广元市售果蔬中BPs的污染状况,发现污染物主要为双酚A和双酚S,检出率分别为80.0%和47.5%,浓度分别在未检出~31.84μg/kg和未检出~15.75μg/kg之间。本方法可用于果蔬中8种BPs的快速提取、净化、定性与定量检测,具有操作简单、灵敏度高、成本低和绿色环保等优势,适合于大批量果蔬中8种双酚类化合物的日常筛查与确证。A method for rapid determination of eight kinds of BPs in fruits and vegetables based on QuEChERS combined with ultra-high performance liquid chromatography-tandem mass spectrometry(UPLC-MS/MS)was developed.The effects of matrix effect(ME)and extraction recovery(RE)on process efficiency(PE)were discussed.Approximately 10.00 g of homogeneous fruit and vegetable samples were accurately weighed,and 10 mL of acetonitrile and 1.0 g of NaAC were added for extraction,respectively.And then,2 mL of organic phase was taken into a 15-mL centrifuge tube,and the mixed purifier(33 mg PSA,33 mg GCB and 10 mg C_(18))was added for purification.After centrifugation,0.5 mL of supernatant was added into 0.5 mL of methanol aqueous solution(50%,V/V),and the mixture was analyzed by UPLC-MS/MS.The chromatographic separation was performed on a Waters BEH C_(18)(100 mm×2.1 mm,1.7μm)column using methanol and 0.1 mmol/L ammonium bicarbonate aqueous solution as mobile phase.Quantitative analysis was performed by isotope internal standard method in the modes of electrospray ionization,anion and multiple reaction monitoring.The results showed that the chromatographic separation of eight kinds of BPs could be completed within 8 min with good linearity and correlation coefficients(R^(2)>0.9990).The limits of detection(LODs)and limits of quantification(LOQs)ranged from 0.01 to 0.10μg/kg and 0.03 to 0.35μg/kg,respectively.The average recoveries of eight kinds of BPs in different fruits and vegetables were 67.2%-117.8%with relative standard deviations(RSDs)of 0.1%-8.3%.This method was used to detect BPs in fruits and vegetables from Guangyuan city,and it bisphenol A and bisphenol S were found to be the main contaminants with the detection rates of 80.0%and 47.5%,respectively.The concentrations of bisphenol A and bisphenol S ranged from not detected to 31.84μg/kg and from not detected to 15.75μg/kg,respectively.This method could rapidly extract,purify and quantitatively detect eight kinds of BPs in fruits and vegetables with the advantages suc

关 键 词：QUECHERS 超高效液相色谱-三重四极杆串联质谱 双酚类物质 果蔬 

分 类 号：O657.63[理学—分析化学] TS255.7[理学—化学]