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Quantifying Inorganic Arsenic and Other Water-Soluble Arsenic Species in Human Milk by HPLC/ICPMS
Analytical Chemistry ( IF 6.7 ) Pub Date : 2017-04-29 00:00:00 , DOI: 10.1021/acs.analchem.7b01276
Michael Stiboller 1 , Georg Raber 1 , Elin Lovise Folven Gjengedal 2 , Merete Eggesbø 3 , Kevin A. Francesconi 1
Analytical Chemistry ( IF 6.7 ) Pub Date : 2017-04-29 00:00:00 , DOI: 10.1021/acs.analchem.7b01276
Michael Stiboller 1 , Georg Raber 1 , Elin Lovise Folven Gjengedal 2 , Merete Eggesbø 3 , Kevin A. Francesconi 1
Affiliation
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Because the toxicity of arsenic depends on its chemical form, risk assessments of arsenic exposure must consider the type of arsenic compound, and hence they require sensitive and robust methods for their determination. Furthermore, the assessment should include studies on the most vulnerable people within a population, such as newborns and infants, and thus there is a need to quantify arsenic species in human milk. Herein we report a method for the determination of arsenic species at low concentrations in human milk by HPLC/ICPMS. Comparison of single and triple quadrupole mass analysers showed comparable performance, although the triple quadrupole instrument more efficiently overcame the problem of ArCl+ interference, from the natural chloride present in milk, without the need for gradient elution HPLC conditions. The method incorporates a protein precipitation step with trifluoroacetic acid followed by addition of dichloromethane or dibromomethane to remove the lipids. The aqueous phase was subjected to anion-exchange and cation-exchange/mixed mode chromatography with aqueous ammonium bicarbonate and pyridine buffer solutions as mobile phases, respectively. For method validation, a human milk sample was spiked with defined amounts of dimethylarsinate, arsenobetaine, and arsenate. The method showed good recoveries (99–103%) with detection limits (in milk) in the range of 10 ng As kg–1. The method was further tested by analyzing two Norwegian human milk samples where arsenobetaine, dimethylarsinate, and a currently unknown As species were found, but iAs was not detected.
中文翻译：
通过HPLC / ICPMS定量测定母乳中的无机砷和其他水溶性砷
由于砷的毒性取决于其化学形式，因此对砷暴露的风险评估必须考虑砷化合物的类型，因此它们需要灵敏而稳健的测定方法。此外，评估应包括对人口中最脆弱的人群（如新生儿和婴儿）进行的研究，因此有必要对人乳中的砷种类进行量化。本文中，我们报告了一种通过HPLC / ICPMS测定人乳中低浓度砷物种的方法。尽管三重四极杆质谱仪更有效地克服了ArCl +的问题，但单重和三重四极杆质量分析仪的比较显示了可比的性能。不受牛奶中天然氯化物的干扰，而无需使用梯度洗脱HPLC条件。该方法包括用三氟乙酸沉淀蛋白质的步骤，然后加入二氯甲烷或二溴甲烷以除去脂质。将水相进行阴离子交换和阳离子交换/混合模式色谱分析，分别以碳酸氢铵水溶液和吡啶缓冲溶液为流动相。为了进行方法验证，在人乳样品中掺入了规定量的二甲基砷酸二甲酯，砷基甜菜碱和砷酸二甲酯。该方法显示出良好的回收率（99–103％），检出限（牛奶中）为10 ng As kg –1。通过分析两个挪威人乳样品进一步测试了该方法，其中发现了砷甜菜碱，二甲基砷酸和目前未知的As物种，但未检测到iAs。
更新日期：2017-05-11
中文翻译：
通过HPLC / ICPMS定量测定母乳中的无机砷和其他水溶性砷
由于砷的毒性取决于其化学形式，因此对砷暴露的风险评估必须考虑砷化合物的类型，因此它们需要灵敏而稳健的测定方法。此外，评估应包括对人口中最脆弱的人群（如新生儿和婴儿）进行的研究，因此有必要对人乳中的砷种类进行量化。本文中，我们报告了一种通过HPLC / ICPMS测定人乳中低浓度砷物种的方法。尽管三重四极杆质谱仪更有效地克服了ArCl +的问题，但单重和三重四极杆质量分析仪的比较显示了可比的性能。不受牛奶中天然氯化物的干扰，而无需使用梯度洗脱HPLC条件。该方法包括用三氟乙酸沉淀蛋白质的步骤，然后加入二氯甲烷或二溴甲烷以除去脂质。将水相进行阴离子交换和阳离子交换/混合模式色谱分析，分别以碳酸氢铵水溶液和吡啶缓冲溶液为流动相。为了进行方法验证，在人乳样品中掺入了规定量的二甲基砷酸二甲酯，砷基甜菜碱和砷酸二甲酯。该方法显示出良好的回收率（99–103％），检出限（牛奶中）为10 ng As kg –1。通过分析两个挪威人乳样品进一步测试了该方法，其中发现了砷甜菜碱，二甲基砷酸和目前未知的As物种，但未检测到iAs。
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