气相色谱-质谱联用测定母乳中合成麝香

建立了凝胶渗透色谱(GPC)柱和硅胶柱净化,气相色谱-质谱(GC/MS)测定母乳中合成麝香的分析方法.实验结果表明:GC/MS在0.01μg.ml-1到1μg.ml-1的浓度范围内对4种常见合成麝香(佳乐麝香HHCB、吐纳麝香AHTN、二甲苯麝香MX和酮麝香MK)均有良好的线性响应,4种合成麝香的基质加标回收率为76%—115%,相对标准偏差为2.8%—7.4%.利用信噪比(5/1)确定该方法的定性检测限,HHCB,AHTN,MX为5ng.g-1脂重,MK为4ng.g-1脂重,定量检测限为定性检测限的2倍.采用上述方法分析了上海母乳样品中合成麝香的浓度和分布特征,发现母乳中普遍存在这4种合成麝香,浓度分别为HHCB92±70;AHTN16±12;MX26±22;MK16±14ng.g-1脂重,与欧美国家的污染水平相比,总体含量偏低.

DETERMINATION OF SYNTHETIC MUSKS IN HUMAN MILK SAMPLES BY GAS CHROMATOGRAPHY/MASS SPECTROMETRY

Synthetic musk fragances are considered as new emerging environmental contaminants in the category of Pharmaceuticals and Personal Care Products.In this paper,the detection method of synthetic musk using gas chromatography and mass spectrometry(GC/MS)was developed.Gel permeation chromatography(GPC)and silica gel packed column were introduced as cleanup procedures.The linear ranges for HH_cB,AHTN,MX and MK were 0.01-1.0μg·ml~(-1).The recovery rate of spiked samples was 76%-115%,and RSD was 2.8%-7.4%.Phenanthrene-d10 was used as a surrogate and the recovery was 81%-113%.The limit of detection(LODs)and limit of quantification(LOQs)were based on a signal-to-noise ratio of 5 and 10,respectively.The LOD was 5ng·g~(-1) lipid weight for HH_cB,AHTN,MX and 4 ng·g~(-1) lipid weight for MK,respectively.Using this method,the concentration of synthetic musks in ten human milk samples from shanghai was detected.The results show that the occurrence of synthetic musks is common.The mean concentrations were HH_cB 92±70; AHTN 16±12 ; MX 26±22; MK 16±14 ng·g~(-1) lipid weight.The contamination level is lower than those reported in EU and USA.