气相色谱-串联质谱法测定婴儿奶粉中16种邻苯二甲酸酯类化合物  

Determination of 16 phthalate acid esters in infant formula by gas chromatography-tandem mass spectrometry

作　　者：许兵兵 李晓敏[2] 张庆合[2] 朱维晃[1] XU Bingbing;LI Xiaomin;ZHANG Qinghe;ZHU Weihuang(School of Environmental and Municipal Engineering,Xi’an University of Architecture&Technology, Xi’an 710055,China;Division of Chemical Metrology and Analytical Science, National Institute of Metrology,Beijing 100029,China)

机构地区：[1]西安建筑科技大学环境与市政工程学院,陕西西安710055 [2]中国计量科学研究院化学计量与分析科学研究所,北京100029

出　　处：《色谱》2018年第8期786-794,共9页Chinese Journal of Chromatography

基　　金：中国计量科学研究院基本科研业务费专项(21-AKY1619)~~

摘　　要：建立了气相色谱-串联质谱(GC-MS/MS)测定复杂基体婴儿奶粉中16种邻苯二甲酸酯类塑化剂的分析方法。奶粉样品以水溶解均质,乙腈提取,乙二胺-N-丙基硅烷(PSA)类型玻璃固相萃取柱净化,DB-5 MS UI气相色谱柱(30 m×0.25 mm×0.25μm)分离,同位素稀释质谱法(IDMS)定量。比较了氧化铝/PSA和PSA两种固相萃取柱在不同洗脱条件下萃取16种塑化剂的回收率。最终选择PSA固相萃取柱,以正己烷-丙酮(60∶40,v/v)作为洗脱溶剂,实现奶粉基体中16种塑化剂的净化。采用基质匹配同位素内标法定量,16种塑化剂在0.01~2.0m g/kg范围内线性良好,线性相关系数(R2)大于0.999 6,检出限和定量限分别是0.15~2.50μg/kg和0.50~8.33μg/kg,加标回收率为96.1%~104.0%,相对标准偏差(RSD)小于3.3%(n=5),该方法灵敏度好、精密度高,适用于婴儿奶粉基体中16种塑化剂的痕量分析。A method was established for the determination of 16 phthalate acid esters(PAEs)in infant formula by gas chromatography-tandem mass spectrometry(GC-MS/MS).PAEs in infant formula samples were homogenized by deionized water,extracted with acetonitrile,and purified by a solid-phase extraction(SPE)method using primary secondary amine(PSA)sorbents.The separation was performed on a DB-5 MS UI(30 m×0.25 mm×0.25μm)capillary column.Effects of different elution solvents on alumina/PSA and PSA SPE columns were investigated.Fair recoveries of 16 PAEs were achieved on the PSA column upon elution by mixed n-hexane-acetone(60∶40,v/v).All the 16 PAEs were quantified by matrix-matched isotopic-dilution mass spectrometry(IDMS);the 16 PAEs showed linear relationships in the concentration range of 0.01-2.0 mg/kg with linear coefficients(R 2)greater than 0.999 6.The limits of detection(LODs)and quantification(LOQs)were in the range of 0.15-2.5μg/kg and 0.50-8.33μg/kg,respectively.The recoveries of the 16 PAEs,obtained using the IDMS method,were 96.1%-104.0%with relative standard deviations(RSDs)lower than 3.3%(n=5).These results established the method described here as sensitive and precise for the simultaneous determination of 16 PAEs in infant formula,even at trace concentrations.

关 键 词：气相色谱-串联质谱 同位素稀释质谱法 固相萃取 邻苯二甲酸酯类塑化剂 婴儿奶粉 

分 类 号：O658[理学—分析化学]