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Phosphorus-specific determination of glyphosate, glufosinate, and their hydrolysis products in biological samples by liquid chromatography-inductively coupled plasma-mass spectrometry

机译:液相色谱-电感耦合等离子体质谱法测定磷在生物样品中的草甘膦,草铵膦及其水解产物

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Anion exchange liquid chromatography (LC) with inductively coupled plasma-mass spectrometry (ICP-MS) was used for simultaneous determination of gly-phosate and glufosinate (phosphonic and amino acid group-containing herbicides; PAAHs) and their hydrolysis products, aminomethylphosphonic acid (AMPA) and 3-meth-ylphosphinicoacetic acid (MPPA), in biological samples. The target compounds were separated using an anion exchange resin column and gradient elution with sodium carbonate and sodium hydroxide system. The chromato-graphic eluates were passed through a membrane suppressor system and monitored by phosphorus-specific detection at ml z 31. PAAHs and their hydrolysis products were baseline separated from each other within 40 min of elution time, and phosphoric acid did not interfere with detection. The detection limits in serum samples were 0.1-0.7 ug/ml; those in urine samples, 0.2-1.6 jig/ml for the four compounds. The spiked recoveries for the four compounds were over 91 % in serum and urine samples. The detection of the compounds was not subject to interference from sample matrix components. The present method would be useful for toxicological analysis of PAAHs and their products in actual forensic practice. To our knowledge, this is the first trial to establish an LC-ICP-MS method for analysis of PAAHs and their products in biological samples .
机译:阴离子交换液相色谱(LC)和电感耦合等离子体质谱(ICP-MS)用于同时测定草甘膦和草铵膦(含膦酸和氨基酸基团的除草剂; PAAH)及其水解产物氨基甲基膦酸(生物样品中的AMPA)和3-甲基-基次膦基乙酸(MPPA)。使用阴离子交换树脂柱分离目标化合物,并用碳酸钠和氢氧化钠体系进行梯度洗脱。色谱洗脱液通过膜抑制器系统,并通过磷特异性检测在ml z 31处进行监测。PAAH及其水解产物在洗脱时间内40分钟内彼此基线分离,磷酸不干扰检测。血清样品的检出限为0.1-0.7 ug / ml;尿样中的那些化合物,四种化合物的浓度为0.2-1.6夹具/毫升。血清和尿液样品中四种化合物的加标回收率均超过91%。化合物的检测不受样品基质组分的干扰。本方法可用于实际法医实践中对PAAHs及其产品的毒理学分析。据我们所知,这是建立LC-ICP-MS方法用于分析生物样品中PAAH及其产物的第一个试验。

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