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HPLC-accelerator MS measurement of atrazine metabolites in human urine after dermal exposure

机译:皮肤暴露后高效液相色谱-加速器质谱法测定人尿中阿特拉津的代谢产物

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Metabolites of atrazine were measured in human urine after dermal exposure using HPLC to separate and identify metabolites and accelerator mass spectrometry (AMS) to quantify them, Ring-labeled [C-14]atrazine was applied for 24 h with a dermal patch to human volunteers at low (0.167 mg, 6.45 mu Ci) and high (1.98 mg, 24.7 mu Ci) doses. Urine was collected for 7 days. The mine was centrifuged to remove solids, and the supernatant was measured by liquid scintillation counting prior to injection on the HPLC to ensure that <0.17 Po (4.5 pCi) was injected on the column. A reversed-phase gradient of 0.1% acetic acid in water and 0.1% acetic acid in acetonitrile became less polar with increasing time and separated the parent compound and major atrazine metabolites over 31 min on an octadecylsilane column. Peaks were identified by coelution with known standards. Elution fractions were collected in 1-min increments; half of each fraction was analyzed by AMS to obtain limits of quantitation of 14 amol. Mercapturate metabolites of atrazine and dealkylated atrazine dominated the early metabolic time points, accounting for similar to 90% of the 14C in the urine. No parent compound was detected. The excreted atrazine metabolites became:more polar with increasing time, and an unidentified polar metabolite that was present in all samples became as prevalent as any of the known ring metabolites several days after the dose was delivered. Knowledge of metabolite dynamics is crucial to developing useful assays for monitoring atrazine exposure in agricultural workers. [References: 25]
机译:皮肤接触后,使用HPLC测定人尿中阿特拉津的代谢产物,以分离和鉴定代谢产物,并通过加速器质谱(AMS)对其进行定量,将环标记的[C-14]阿特拉津与皮肤贴剂一起应用24小时,用于志愿者低剂量(0.167 mg,6.45 mu Ci)和高剂量(1.98 mg,24.7 mu Ci)。收集尿液7天。将矿井离心去除固体,在注入HPLC前通过液体闪烁计数法测量上清液,以确保将<0.17 Po(4.5 pCi)注入色谱柱。随着时间的延长,水中0.1%的乙酸和乙腈中的0.1%乙酸的反相梯度会变得极性降低,并在十八烷基硅烷色谱柱上经过31分钟分离出母体化合物和主要的at去津代谢物。通过与已知标准品的共同洗脱鉴定峰。以1分钟为增量收集洗脱级分;通过AMS分析每个馏分的一半以获得14 amol的定量限。阿特拉津和脱烷基阿特拉津的巯基代谢产物在早期代谢时间点占主导地位,约占尿液中14 C的90%。未检测到母体化合物。排出的at去津代谢物变为极性:随着时间的增加,极性增强;在给药后数天,所有样品中存在的未知极性代谢物与任何已知的环状代谢物一样普遍。代谢物动力学的知识对于开发用于监测农业工人中r去津暴露的有用测定至关重要。 [参考:25]

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