超高效液相色谱-串联质谱法检测动物源性食品中8种有机磷酸酯  

Determination of eight organophosphate esters in animal-derived foods by ultra performance liquid chromatography-tandem mass spectrometry

作　　者：唐艳 闻胜[2] 曹文成 刘潇[2] 雷承霖 程青云 陈海川 刘翎 刘小方[2] 周妍[2] TANG Yan;WEN Sheng;CAO Wencheng;LIU Xiao;LEI Chenglin;CHENG Qingyun;CHEN Haichuan;LIU Ling;LIU Xiaofang;ZHOU Yan(College of Life Sciences and Technology,Xinjiang University,Urumqi 830017,China;NHC Specialty Laboratory of Food Safety Risk Assessment and Standard Development,Hubei Provincial Center for Disease Control and Prevention,Wuhan 430079,China;School of Life and Health Sciences,Hubei University Of Technology,Wuhan 430079,China)

机构地区：[1]新疆大学生命科学与技术学院,新疆乌鲁木齐830017 [2]国家卫生健康委员会食品安全风险评估与标准研制特色实验室,湖北省疾病预防控制中心,湖北武汉430079 [3]湖北工业大学生命科学与健康工程学院,湖北武汉430079

出　　处：《色谱》2025年第4期309-316,共8页Chinese Journal of Chromatography

基　　金：国家重点研发计划(2023YFF1104800);湖北省自然科学基金项目(2022CFB022,2023AFB1012,2024AFB526);湖北省卫生健康委科研资助(WJ2023M106).

摘　　要：采用乙腈作为提取溶剂,结合超声波辅助萃取和SPE柱进行前处理,建立了超高效液相色谱-串联质谱测定动物源性食品中8种有机磷酸酯(OPEs)的检测方法。准确称取0.5 g样品,用5 mL乙腈超声萃取;冷冻离心后取上清液,用HMR-Lipid SPE柱进行净化,待测分析物经C 18色谱柱分离,在正离子模式下采集,2,2-二(氯甲基)-1,3-丙二醇双[双(2-氯乙基)磷酸酯]酯(V6)采用外标法定量,其他7种化合物(磷酸三乙酯(TEP)、磷酸三丙酯(TPrP)、磷酸三丁酯(TnBP)、磷酸三(2-氯乙基)酯(TCEP)、磷酸三(2-氯丙基)酯(TCIPP)、磷酸三(1,3-二氯-2-丙基)酯(TDCIPP)和磷酸三苯酯(TPHP))采用内标法定量。结果表明,该方法线性相关系数r 2≥0.9900;各物质检出限为0.01~0.87μg/kg,定量限为0.02~2.62μg/kg;在2、20、100μg/kg 3个水平下进行加标回收试验,回收率为80.5%~117.8%;RSD≤14.8%(n=6)。按此方法分析了12种动物源性食品样品(草鱼、鲈鱼、小龙虾、牛乳、奶粉、酸奶、猪肉、牛肉、鸡肉、鸭肉、鸡蛋和鸭蛋),其中化合物TnBP和TCIPP的检出率为100%,TEP、TCEP、TPHP和TDCIPP的检出率高于50%,TPrP和V6未检出。本方法前处理操作简单,分析速度快,回收率和精密度较好,适用于多种动物源性食品中OPEs的快速分析检测。Organophosphate esters(OPEs)are widely used as flame retardants in most regions,they adversely affect ecosystems and threaten human health.OPEs have attracted significant public attention because they are toxic and ubiquitously present in the environment.While China is among the world’s largest users and producers of OPEs,limited data on the exposure of animal-derived foods to OPEs exist;consequently,a method for quantifying OPEs in animal-derived food samples is needed.In this study,a method was developed for the determination of eight OPEs,including triethyl phosphate(TEP),tripropyl phosphate(TPrP),tri-n-butyl phosphate(TnBP),tris(2-chloroethyl)phosphate(TCEP),tris(2-chloroisopropyl)phosphate(TCIPP),tris(1,3-dichloro-2-propyl)phosphate(TDCIPP),triphenyl phosphate(TPHP),and 2,2-bis(chloromethyl)trimethylene bis[bis(2-chloroethyl)phosphate](V6),from twelve types of typical animal-derived foods by ultra performance liquid chromatography-tandem mass spectrometry(UPLC-MS/MS).The samples were purified using an HMR-Lipid SPE column.The effects of mobile phase A(water,5 mmol/L ammonium acetate aqueous solution,and 0.1%formic acid aqueous solution)and mobile phase B(methanol and acetonitrile),as well as the methanol/acetonitrile ratio on the separation and extraction efficiencies for the eight OPEs were investigated using one-way analysis.The results showed that optimal response values and peak shapes were obtained for the various compounds using 0.1%formic acid aqueous solution-acetonitrile system as the mobile phase.The following pretreatment procedure was used:A 0.5 g sample was accurately weighed and ultrasonically extracted with 5 mL of acetonitrile.The supernatant was collected after freezing and centrifugation,and cleaned-up was performed using an HMR-Lipid SPE column.The target analytes were analyzed using a Waters Acquity BEH C 18 column(100 mm×2.1 mm,1.7μm)and ESI+MS conditions.Compound V6 was quantified by the external standard method,with the other seven compounds quantified using the internal standard m

关 键 词：有机磷酸酯 动物源性食品 超高效液相色谱-串联质谱 

分 类 号：O658[理学—分析化学]