Determination of phthalate monoesters in human milk, consumer milk, and infant formula by tandem mass spectrometry (LC–MS–MS)
Determination of phthalate monoesters in human milk, consumer milk, and infant formula by tandem mass spectrometry (LC–MS–MS)
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DOI：
10.1007/s00216-005-3218-0
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发表时间：
2005-06
影响因子：
4.3
通讯作者：
G. K. Mortensen;K. Main;A. Andersson;H. Leffers;N. Skakkebæk
中科院分区：
文献类型：
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作者：
G. K. Mortensen;K. Main;A. Andersson;H. Leffers;N. Skakkebæk
人类每天接触邻苯二甲酸盐可能会对健康造成风险，因为动物实验表明这些化合物会影响生殖系统的分化和功能。由于牛奶是婴儿的主要营养来源，邻苯二甲酸酯水平的知识对于暴露和风险评估非常重要。在这里，我们描述了一种定量分析方法的开发和验证，用于测定人乳中的邻苯二甲酸酯代谢物。研究的邻苯二甲酸单酯为：邻苯二甲酸单甲酯（mMP）、邻苯二甲酸单乙酯（mEP）、邻苯二甲酸单正丁酯（mBP）、邻苯二甲酸单苄酯（mBzP）、邻苯二甲酸单（2-乙基己基）酯（mEHP）和邻苯二甲酸单异壬酯（mNP）。该方法基于用乙酸乙酯和环己烷（95：5）的混合物进行液体萃取，然后进行两步固相萃取（SPE）。通过使用Betasil苯基柱（100 mm×2.1 mm×3 μm）的高压液相色谱法和三重串联质谱法（LC-MS-MS）完成邻苯二甲酸单酯的检测和定量。检测限在0.01至0.5 μg L− 1范围内，方法变异性为5%至15%。对36个牛奶样本的分析表明，所有这些邻苯二甲酸酯都存在，尽管浓度不同。获得的中位值（μg L−1）分别为0.11（mMP）、0.95（mEP）、3.5（mBP）、0.8（mBzP）、9.5（mEHP）和101（mNP）。我们还分析了7个消费者牛奶样本和10个婴儿配方奶粉样本。在这些样本中仅检测到mBP和mEHP，范围为0.6-3.9 μg L−1（mBP）和5.6-9.9 μg L−1（mEHP）。
Daily exposure of humans to phthalates may be a health risk because animal experiments have shown these compounds can affect the differentiation and function of the reproductive system. Because milk is the main source of nutrition for infants, knowledge of phthalate levels is important for exposure and risk assessment. Here we describe the development and validation of a quantitative analytical procedure for determination of phthalate metabolites in human milk. The phthalate monoesters investigated were: monomethyl phthalate (mMP), monoethyl phthalate (mEP), mono-n-butyl phthalate (mBP), monobenzyl phthalate (mBzP), mono-(2-ethylhexyl) phthalate (mEHP), and monoisononyl phthalate (mNP). The method is based on liquid extraction with a mixture of ethyl acetate and cyclohexane (95:5) followed by two-step solid-phase extraction (SPE). Detection and quantification of the phthalate monoesters were accomplished by high-pressure liquid chromatography using a Betasil phenyl column (100 mm×2.1 mm×3 μm) and triple tandem mass spectrometry (LC–MS–MS). Detection limits were in the range 0.01 to 0.5 μg L−1and method variation was from 5 to 15%. Analysis of 36 milk samples showed that all these phthalates were present, albeit at different concentrations. Median values (μg L−1) obtained were 0.11 (mMP), 0.95 (mEP), 3.5 (mBP), 0.8 (mBzP), 9.5 (mEHP), and 101 (mNP). We also analysed seven samples of consumer milk and ten samples of infant formula. Only mBP and mEHP were detected in these samples, in the ranges 0.6–3.9 μg L−1(mBP) and 5.6–9.9 μg L−1(mEHP).