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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。
OBJECTIVE To determine the residual levels of 10 common phthalate esters (PAEs) metabolites in the urine of infants and young children by using improved HLB cartridge purification and high performance liquid chromatography-tandem mass spectrometry (HPLCMS / MS). Methods A total of 50 cases of infants aged 0-6 months were recruited. The way of feeding infant was surveyed by questionnaire and urine was collected by diapers. The urine was enzymatically hydrolyzed by β-glucuronidase, and the HLB column was purified and concentrated. The urine was separated on a Hypersil Gold Phenyl column (1.9 μm, 100 mm × 2.1 mm), detected by electrospray ionization mass spectrometry and quantified by isotope internal standard method. Results The limit of detection (LOD) of 10 phthalate metabolites was 0.06 ~ 0.16μg / L, and the correlation coefficient (R ~ 2) was greater than 0.99 and 5.0 ~ 50μg / L within the linear range of 0.2 ~ 500μg / L The spiked recoveries were between 82% and 116% with relative standard deviations (RSD, n = 5) of 1.5% to 12.2%. The detection rates of eight phthalates metabolites in urine of infants and young children were 98 %, The geometric mean concentration (μg / L) descending order of monoisobutyl phthalate (MiBP, 10.35), mono , 5.13), butylphthalate (MBP, 4.53), ethyl phthalate (MEP, 1.98), methylphthalate (MMP, 1.69), 2-ethylhexylphthalate (MEHP, 1.22), 2-ethyl-5-carbonylhexyl phthalate (MEHHP, 1.18) and 2-ethyl-5-oxyhexyl phthalate ), MBzP and MCHP were lower (28% and 2%, respectively). Milk powder feeding may be the infant endocrine disruptors di (2-ethylhexyl) phthalate (DEHP, a parent compound of MEHP, MEOHP, MEHHP and MECPP) and butylbenzyl phthalate (BBzP, MBzP parent compound) one of the main ways of exposure. Conclusion HLB column purification-HPLC-MS / MS can be used to accurately determine the metabolites of 10 kinds of PAEs in urine of infants and young children. It can be further used to evaluate the risk of PAEs exposure in infants and young children.