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验证分析方法在尿液和羊粪便中检测氯丹及其代谢物。

Validation of analytical methods for chlordecone and its metabolites in the urine and feces of ewes.

机构信息

UR AFPA - INRA USC 340 - Université de Lorraine, 2 avenue de la Forêt de Haye -TSA 40602, 54518 Vandœuvre-lès-Nancy Cedex, France.

Université de Paris-Est, ANSES, Laboratory for Food Safety, F 94700 Maisons-Alfort, France.

出版信息

J Chromatogr B Analyt Technol Biomed Life Sci. 2018 Sep 1;1093-1094:66-76. doi: 10.1016/j.jchromb.2018.06.058. Epub 2018 Jul 3.

Abstract

Chlordecone (CLD) is a Persistent Organic Pollutant used between 1972 until 1993 in the French West Indies (FWI). Due to its persistence and extensive application, a quarter of the total local agricultural acreage is still moderate to heavily polluted. In consequence, livestock may be contaminated at various levels. This is a major public health concern, particularly for local consumers. In order to better understand the fate of CLD in livestock organisms, in vivo studies are required. There is no information available about its metabolism and elimination in ruminants, common livestock in the FWI. To be able to monitor the fate of chlordecone and its metabolites in livestock and to assess if the compounds could be released in the environment, urinary and fecal samples were logically targeted. In order to reach this goal, robust and validated analytical methods are required. For this purpose, Quick, Easy, Cheap, Effective, Rugged, and Safe (QuEChERS) extraction methods were validated to analyze CLD and its metabolites in the urine and feces. The analysis was carried using liquid phase chromatography with tandem mass spectrometry and validated according to French standard NF V03-110 and SANTE guidelines. Matrix effect, Accuracy, within-laboratory repeatability, specificity, Q/q relative ion intensities and uncertainty were reported. Recoveries between 70% and 120% were obtained from urine and feces. The limits of quantification (LOQ) in urine samples were 0.1 μg CLD L, 0.1 μg total CLD (CLD and its conjugates)·L, 1.3 μg CLDOH L and 2.4 μg total CLD (chlordecol and its conjugates) L of urine. LOQ in fresh feces were 3.2 μg CLD kg and 5.8 μg CLDOH kg. Contaminated urinary and fecal samples from ewes were analyzed to confirm the relevance of the methods. In urine, CLD and conjugated CLDOH could be quantified whereas only free CLD and free CLDOH were found in feces. These methods are essential for future toxicokinetic studies and also to estimate the environmental contamination.

摘要

氯丹(CLD)是一种持久性有机污染物,1972 年至 1993 年在法属西印度群岛(FWI)使用。由于其持久性和广泛应用,四分之一的当地农业用地仍受到中度至重度污染。因此,牲畜可能在不同层面受到污染。这是一个主要的公共卫生问题,特别是对当地消费者而言。为了更好地了解 CLD 在牲畜体内的命运,需要进行体内研究。关于其在 FWI 常见牲畜反刍动物中的代谢和消除,目前尚无信息。为了能够监测氯丹及其代谢物在牲畜中的命运,并评估这些化合物是否可能释放到环境中,尿液和粪便样本是合乎逻辑的目标。为了实现这一目标,需要稳健和经过验证的分析方法。为此,采用快速、简便、廉价、有效、耐用和安全(QuEChERS)提取方法对尿液和粪便中的 CLD 和其代谢物进行了验证分析。该分析采用液相色谱-串联质谱法进行,并根据法国标准 NF V03-110 和 SANTE 指南进行了验证。报告了基质效应、准确度、实验室内部重复性、特异性、Q/q 相对离子强度和不确定度。从尿液和粪便中获得了 70%至 120%的回收率。尿液样本的定量限(LOQ)分别为 0.1μg CLD·L、0.1μg 总 CLD(CLD 和其轭合物)·L、1.3μg CLDOH·L 和 2.4μg 总 CLD(氯癸醇和其轭合物)·L。新鲜粪便中的 LOQ 分别为 3.2μg CLD·kg 和 5.8μg CLDOH·kg。对来自母羊的受污染尿液和粪便样本进行了分析,以确认方法的相关性。在尿液中,可以定量测定 CLD 和结合的 CLDOH,而在粪便中仅发现游离的 CLD 和游离的 CLDOH。这些方法对于未来的毒代动力学研究以及估计环境污染也至关重要。

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