HLB固相萃取-高效液相色谱串联质谱法测定婴幼儿尿液中邻苯二甲酸酯代谢物

发布时间：2018-06-27 16:56

本文选题：邻苯二甲酸酯 + 婴幼儿　；参考：《卫生研究》2017年04期

【摘要】：目的利用改进的HLB小柱净化和高效液相色谱-串联质谱法(HPLCMS/MS)测定10种常见的邻苯二甲酸酯(PAEs)代谢物在婴幼儿人群尿液中的残留水平。方法征集了50例0~6月龄普通婴幼儿,通过问卷调查了婴儿的喂养方式,利用纸尿裤采集其尿液。尿液经β-葡萄糖醛酸酶酶解、HLB柱净化浓缩后,采用Hypersil Gold Phenyl色谱柱(1.9μm,100 mm×2.1 mm)分离,电喷雾电离质谱检测,同位素内标法定量。结果 10种邻苯二甲酸酯代谢物检出限(LOD)为0.06~0.16μg/L,在0.2~500μg/L线性范围内相关系数(R~2)均大于0.99,5.0~50μg/L加标水平下回收率为82%~116%,相对标准偏差(RSD,n=5)为1.5%~12.2%;婴幼儿尿液中8种邻苯二甲酸酯代谢物检出率在98%以上,几何平均浓度(μg/L)从高到低依次为邻苯二甲酸单异丁酯(MiBP,10.35)、邻苯二甲酸单(5-羰基-2-己戊基)酯(MECPP,5.13)、邻苯二甲酸丁酯(MBP,4.53)、邻苯二甲酸乙酯(MEP,1.98)、邻苯二甲酸甲酯(MMP,1.69)、邻苯二甲酸(2-乙基己基)酯(MEHP,1.22)、邻苯二甲酸(2-乙基-5-羰基己基)酯(MEHHP,1.18)和邻苯二甲酸(2-乙基-5-氧己基)酯(MEOHP,0.99),邻苯二甲酸苄基酯(MBzP)和邻苯二甲酸单环己酯(MCHP)检出率较低(分别为28%和2%)。奶粉喂养可能是婴儿内分泌干扰物邻苯二甲酸二(2-乙基)己酯(DEHP,是MEHP、MEOHP、MEHHP和MECPP的母体化合物)和邻苯二甲酸丁基苄基酯(BBzP,是MBzP的母体化合物)暴露的主要途径之一。结论利用HLB柱净化-HPLC-MS/MS技术可准确测定婴儿尿液中10种长短链PAEs代谢物,可以进一步用于婴幼儿人群的PAEs暴露风险评估。
[Abstract]:Objective to determine the residual levels of 10 common metabolites of phthalates (PAEs) in urine of infants by improved HLB column purification and high performance liquid chromatography-tandem mass spectrometry (HPLCMS / MS). Methods 50 normal infants aged 0 to 6 months were collected and their urine was collected by questionnaire. Urine was purified and concentrated by 尾 -glucuronidase hydrolysate HLB column. The urine was separated by Hypersil Gold Phenyl column (1.9 渭 m of 100 mm 脳 2.1 mm). Results the detection limit (LOD) of 10 phthalate metabolites was 0.06 ~ 0.16 渭 g / L, and the correlation coefficient (RG-2) in the linear range of 0.2 ~ 500 渭 g / L was higher than 0.995.0 ~ 50 渭 g / L, the recovery was 82 ~ (116), the relative standard deviation (RSDN ~ (5) was 1.5 ~ (12. 2), and 8 phthalate esters were substituted in infant urine. The detectable rate of thank is over 98%. The geometric mean concentrations (渭 g / L) from high to low are monobutyl phthalate (MiBPn10.35), phthalate monoester (5-carbonyl-2-hexyl) ester (MECPP-5.13), butyl phthalate (MBP) 4.53, ethyl phthalate (MEPN 1.98), methyl phthalate (MMPL 1.69), phthalic acid (2-phthalic acid) (MMP1. 69), butyl phthalate (MBP) 4.53, ethyl phthalate (MEP1. 98), methyl phthalate (MMP1. 69), phthalic acid (2-). The detectable rates of ethyl hexyl) ester (MEHP- 1.22), phthalic acid (2-ethyl-5-carbonyl hexyl) ester (MEHHP- 1.18) and phthalic acid (2-ethyl-5-oxy-hexyl) ester (MEOHP- 0.99), benzyl phthalate (MBzP) and monocyclohexyl phthalate (MCHP) were lower (28% and 2%, respectively). Milk powder feeding may be one of the main routes of exposure to diethyl hexyl phthalate (DEHP-) and Ding Ji benzyl phthalate (BBZP, the parent compound of MEHP- MEOHP- MEHHP and MECPP). Conclusion HPLC-MS / MS / MS technique can be used to determine 10 PAEs metabolites in urine of infants and can be further used to assess the exposure risk of PAEs in infants and infants.
【作者单位】：中国科学院城市环境与健康重点实验室中国科学院城市环境研究所;中国科学院大学;
【基金】：浙江省自然科学基金(No.LY14B070005)
【分类号】：R994.6

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