gc lc法在邻苯二甲酸酯 青霉素类药物和染料检测中的应用研究-application of gc lc method in the detection of phthalates penicillin drugs and dyes.docx

摘要本文主要针对食品和化妆品中三类有毒有害物质的进行了研究，分别对奶粉中邻苯二甲酸酯、牛奶中青霉素类药物和染发剂中染料进行了检测分析。1．采用GC-MS法检测奶粉中的邻苯二甲酸酯，内标法定量。邻苯二甲酸二异壬酯（DINP）检出浓度定为1mg/kg，其余16 种化合物检出浓度均可以定为0.01 mg/kg，检出浓度能满足卫生部规定的邻苯二甲酸酯在食品中的最大残留量要求。全部组分校准曲线相关系数均大于0.998，三个浓度添加量均在线性范围内，且回收率均大于90 %，重复性RSD 均小于10 %。2．选用LC-MS/MS法检测牛奶中青霉素类药物残留。样品用乙腈水溶液提取，HLB固相萃取柱净化，用LC-MS/MS测定，基质外标法峰面积定量。双氯西林检出浓度定为0.10 μg/kg，其余6 种青霉素检出浓度均可以定为0.02 μg/kg，完全能满足我国对牛奶中青霉素类药物残留的限度规定。全部化合物校准曲线的相关系数均大于0.999，添加浓度为10 μg/kg、20 μg/kg、30 μg/kg 的回收率均大于70 %，重复性RSD 均小于10 %。3．利用HPLC-DAD检测染发剂中的染料。样品采用10 %亚硫酸氢钠水溶液-乙醇（1∶1）混合溶液稀释，用冰水浴超声提取。12 种染料检出浓度为19～22μg/g，校准曲线相关系数均大于0.999，添加浓度为2000μg/g、3000μg/g、4000 μg/g的回收率均大于95 %，重复性RSD 均小于4 %。关键词：GC-MS；LC-MS/MS；HPLC-DAD；邻苯二甲酸酯；青霉素类药物；染料IABSTRACTThispapermainlyaimingatthreekinds ofpoisonousandharmfulsubstancesin foodandcosmeticswasstudied，respectively,ofphthalateacidesters(phthalates)in milkpowder,penicillindrugs(penicillins)inmilkanddyesinhairdyeswas determined byanalysis.1．DeterminationofphthalatesinmilkpowderbyGC-MSandinternalstandard method.DINPdetectableconcentrationwas1mg/kg.Theremaining16compounds detectionconcentrationcanbesetat0.01mg/kg,fullyabletomeettheMinistryof Health on maximum residue levels in phthalates requirements. All components of the calibrationcurvecorrelationcoefficientweregreaterthan0.998,thethree concentrationaddingquantitywerewithinthelinearrange,andtherecoveryrates were greater than 90 %.RepeatabilityRSD was less than 10%.2．MilkwasdeterminedbyLC-MS/MSmethodofpenicillinsdrugs.Samples wereextractedwithaqueousacetonitrile,purifiedbyHLBsolid-phaseextraction column.UsingLC-MS/MSdetection,matrixexternalstandardmethod, peakareaforquantitative.Dicloxacillindetectableconcentrationcanbesetat0.10μg/kg.The remaining6compoundsdetectionconcentrationcanbesetat0.02μg/kg,fullyable tomeetthelimitsofourcountryofpenicillinsdrugsinmilkregulations.All componentsofthecalibrationcurveofthecorrelationcoefficientsweregreaterthan 0.999.Addingaconcentrationof10μg/kg,20μg/kg,30μg/kg,andtherecovery rates weregreater than 70%. Repeatabi