《食品工业》2023年第44卷第2期324分析检测固相萃取结合LC/MS-MS法测定奶粉中四溴双酚A綦艳，李锦清*，李聪，黄翠莉广东产品质量监督检验研究院（顺德528300）摘要建立固相萃取(solidphaseextraction,SPE)结合液相色谱-串联质谱法(liquidchromatographytandemmass,LC-MS/MS)测定奶粉中四溴双酚A的分析方法。样品用碱性水溶液溶解,以乙腈提取和沉淀蛋白,提取液经水稀释后用磷酸调节pH＜5,用C18固相萃取柱净化。以甲醇和水为流动相,梯度洗脱,C18色谱柱分离,电喷雾(electrosprayionization,ESI)负离子多反应监测模式(multi-reactionmonitoringmode,MRM)进行检测,采用基质匹配-同位素内标法定量。四溴双酚A在0.2~150μg/L范围内呈良好线性关系(linearcorrelationcoefficient,r)≥0.995;方法检出限(limitofdetection,SLOD)为0.5μg/kg,方法定量限(limitofquantification,SLOQ)为1.5μg/kg;添加水平为1.5,3.0和15.0μg/kg,每个浓度水平平行测定6次,平均加标回收率为92.3%~100.2%,相对标准偏(relativestandarddeviations,SRSD)为6.8%~8.3%。该方法前处理简单、回收率高、准确可靠,适用于奶粉中四溴双酚A的定性定量检测。关键词固相萃取;液相色谱-串联质谱法;奶粉;四溴双酚ADeterminationofTetrabromobisphenolAinMilkPowderbySolidPhaseExtractionCombinedWithLiquidChromatographyTandemMassSpectrometryQIYan,LIJinqing*,LICong,HUANGCuiliGuangdongTestingInstituteofProductQualitySupervision(Shunde528300)AbstractAimtoestablishamethodforthedeterminationoftetrabromobisphenolA(TBBPA)inmilkpowderbysolidphaseextractioncombinedwithliquidchromatographytandemmass(LC-MS/MS).Thesamplewasdissolvedinalkalinesolution,andthenextractedandprecipitatedwithacetonitrile.TheextractsolutionwasdilutedwithwaterandadjustedtopH＜5withphosphoricacid,andthenpurifiedbyC18solidphaseextraction(SPE)column.TheanalytewasseparatedonC18columnusingmethanolandwaterasmobilephaseforgradientelution.Thesamplesweredetectedwithnegativeelectrosprayionizationundermultiplereactionmonitionmode,andquantifiedwithmatrixmatching-isotopeinternalstandardmethod.ThecalibrationcurveofTBBPAshowedgoodlinearrelationshipsintherangeof0.2-150μg/Lwiththelinearcorrelationcoefficientnotlessthan0.995.Thelimitsofdetectionandquantitationof...
