Quantitation of dialkyl phosphate metabolites of organophosphate pesticides in human urine using GC-MS-MS with isotopic internal standards

Quantitation of dialkyl phosphate metabolites of organophosphate pesticides in human urine using GC-MS-MS with isotopic internal standards
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DOI:
10.1093/jat/26.5.245
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发表时间:
2002-07-01
影响因子:
2.5
通讯作者:
Barr, DB
Barr, DB
中科院分区:
医学3区
文献类型:
--
作者:
Bravo, R;Driskell, WJ;Barr, DB

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人类接触有机磷农药可以估计从尿代谢产物的存在。建立了一种同位素稀释气相色谱-串联质谱(GC-MS-MS)联用技术,用于定量测定29种有机磷农药的尿中代谢产物。尿样中加入磷酸二烷基酯的稳定同位素类似物,使用共沸蒸馏蒸发,然后将代谢物化学衍生为各自的氯丙基磷酸酯。将氯丙基磷酸酯浓缩,然后使用GC-MS-MS进行分析。该方法的检测限(LOD)在低至中等皮克每毫升范围内(万亿分之一),变异系数小于20%。使用稳定的同位素类似物作为这些代谢物中每一种的内标物允许最高程度的准确度和精密度。此外,低LOD允许在一般人群研究中使用该方法。
Human exposure to organophosphate pesticides can be estimated from the presence of urinary metabolites. An isotope-dilution gas chromatography-tandem mass spectrometry (GC-MS-MS) method was developed for quantitating the six dialkyl phosphate urinary metabolites of at least 29 organophosphate pesticides. Urine samples were spiked with stable isotope analogues of the dialkyl phosphates, evaporated using azeotropic distillation, followed by chemical derivatization of the metabolites to their respective chloropropyl phosphate esters. The chloropropyl phosphate esters were concentrated and then analyzed using GC-MS-MS. The limits of detection (LODs) of the method were in the low-to-mid picogram-per-milliliter range (parts per trillion) with coefficients of variation of less than 20%. The use of stable isotope analogues as internal standards for each of these metabolites allows for the highest degree of accuracy and precision. Additionally, the low LODs allow the use of this method in general population studies.