血液和尿液中草甘膦的净化富集及检测 |
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引用本文: | 宣宇,;傅得锋,;徐晟捷,;唐磊,;应剑波. 血液和尿液中草甘膦的净化富集及检测[J]. 中国法医学杂志, 2014, 0(6): 566-569 |
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作者姓名: | 宣宇, 傅得锋, 徐晟捷, 唐磊, 应剑波 |
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作者单位: | [1]浙江省公安司法鉴定中心,浙江杭州310009; [2]杭州市公安局刑事科学技术研究所,浙江杭州310004 |
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摘 要: | 目的建立血液、尿液中草甘膦的净化富集及定性定量方法。方法取适量血、尿样品,用80%甲醇水溶液稀释,经Agilent Accu Bond NH2(弱阴离子交换柱)净化富集,用3m L 5%氨水溶液洗脱后进行ESI/LC/MRM对草甘膦的定性及阴离子色谱法(IC)的定量检验分析。结果血液、尿液中草甘膦的IC法检验回收率均大于90%,方法的线性范围均在1-100μg/m L,血检测限为0.1μg/m L,尿液为0.08μg/m L。血液、尿液中草甘膦的LC/MRM的方法检测限均在5ng/m L左右。结论建立的血、尿中草甘膦的前处理方法和LC/MRM定性分析及IC定量分析方法,可满足司法检验要求。
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关 键 词: | 法医毒物分析 草甘膦 LC/MRM IC 血液 尿液 |
Exploration of the glyphosate analysis in the urine and plasma |
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Affiliation: | uan Yu,Fu Defeng,Xu Shengjie,Tang Lei,Ying Jianbo (1.The Forensic Science Institute of Public Security of Zhe Jiang Province, Hangzhou 310009,China; 2. Institute of Criminal Science and Technology of Public Security bureau of Hangzhou Municipal, Hangzhou 310004, China) |
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Abstract: | Objective To establish the qualitative and quantitative methods for the glyphosate in the plasma and urine. Methods Sampled appropriate amount of the urine and plasma,then diluted the samples by 80% methanol water solution,depurated and enriched by the SPE column of Agilent Accu Bond NH2,and eluted by 3m L of 5% hartshorn. At last,the elution solution was qualitative detected by ESI / LC / MRM and quantitative determined by IC. Results The quantitative results by IC were that the recoveries were all greater than 90%,and linearity ranges were all between 1-100μg / m L. The limits of the IC detection was0. 1μg / m L in the blood and 0. 08μg / m L in the urine,respectively. The extraordinary sensitivity which is just 5ng / m L as detectability for glyphosate in both of the plasma and urine by LC / MRM. Conclusion The pretreatment method and the qualitative and quantitative detection methods by LC / MRM and IC respectively for the glyphosate in plasma and urine were suitable to the forensic requirement. |
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Keywords: | forensic toxicological analysis glyphosate LC /MRM IC plasma urine |
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