气相色谱法测定血浆中毒死蜱及其主要代谢产物

郭翔; 谢玉璇; 刘奋; 何坚; 林辉; 郭美琼

doi:10.16369/j.oher.issn.1007-1326.2016.04.004

气相色谱法测定血浆中毒死蜱及其主要代谢产物

深圳市职业病防治院, 广东深圳 518019

基金项目:

国家自然科学基金(编号:81302460)

深圳市科技计划项目(编号:JCYJ20150403091305482)

详细信息

作者简介:
郭翔(1982-),男,硕士,助理研究员、主管医师

中图分类号: O657.71
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- 文章访问数: 172
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- PDF下载量: 19
出版历程
- 收稿日期: 2016-02-25

Determination of chlorpyrifos and its metabolite in plasma by GC

Shenzhen Hospital for Prevention and Treatment of Occupational Diseases, Shenzhen, Guangdong 518019, China

摘要

摘要: 目的建立一种灵敏、准确测定血浆中毒死蜱(chlorpyrifos,CPF)及其主要代谢物3,5,6-三氯-2-吡啶醇(3,5,6-trichloro-2-pyridinol,TCP)的气相色谱(GC)方法。方法取0.5 mL家兔血浆加入乙酸乙酯进行液液萃取,离心后取上层有机相,氮气40℃吹干,残留物加入乙酸乙酯定容后,再加入N-甲基叔丁基二甲基硅基三氟乙酰胺(MTBSTFA),50℃下对TCP进行衍生1 h。样品采用气相色谱仪进行检测,以HP-5毛细管柱分离,电子捕获检测器检测。以待测物质的保留时间定性,外标法峰面积定量。结果 CPF和TCP在8 min内得到良好分离。CPF和TCP的质量浓度在0.01~2.50 mg/L的线性范围内与峰面积相关性良好,相关系数分别为0.999 7和0.999 8;最低检测限均为1 μg/L;精密度RSD均小于10%;加标回收率分别为77.60%~106.16%和72.00%~99.86%。结论此方法灵敏准确,简便可靠,可用于血浆中CPF与TCP的含量分析。
- 毒死蜱 /
- 3,5,6-三氯-2-吡啶醇 /
- 气相色谱 /
- 血浆
+ English
Abstract: Objective To develop a simple and sensitive method for simultaneous determination of chlorpyrifos[O,O-diethyl-O-(3,5,6-trichloro-2-pyridinyl) phosphorothioate,CPF] and its specific metabolite 3,5,6-trichloro-2-pyridinol (TCP) in plasma by GC. Methods Plasma of rabbit (0.50 mL) was extracted by ethylacetate. After purification and centrifugation,the organic layer was evaporated with a stream of nitrogen at 40℃. The residue was dissolved in ethylacetate, and TCP was derivatized for an hour at 50℃ with N-(tert-butyldimethylsilyl)-N-methyltrifluoroacetamide (MTBSTFA). Then the sample was injected into the GC system with HP-5 column and ECD. Qualitative analysis was made by the retention time and quantitative analysis by external standard curve. Results Precise separation of CPF and TCP was achieved within 8 minutes. The relationship between peak areas and concentration showed a good linearity in a range from 0.01 to 2.50 mg/L for both CPF and TCP (r=0.999 7, 0.999 8, respectively). The limits of detection were 1μg/L for both CPF and TCP. Percentage recoveries of this procedure in different matrix were between 77.60%-106.16% for CPF, and between 72.00%-99.86% for TCP. The RSDs of the variation were both lower than 10%. Conclusion This proposed method is simple,reliable and sensitive for simultaneous determination of CPF and its metabolite TCP in plasma samples with satisfactory results.
- chlorpyrifos /
- 3,5,6-trichloro-2-pyridinol /
- GC /
- plasma

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参考文献(10)

[1]	BUSBY-HJERPE A L, CAMPBELL J A, SMITH J N, et al. Comparative pharmacokinetics of chlorpyrifos versus its major metabolites following oral administration in the rat[J]. Toxicology, 2010,268(1/2):55-63.
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施引文献(2)

期刊类型引用(2)

1.	郭翔, 李添娣, 谢玉璇, 何俊涛, 刘奋, 何坚, 林辉, 郭美琼. 优化血液灌流清除毒死蜱及其代谢产物条件的体外实验. 职业卫生与应急救援. 2019(04): 323-327 . 本站查看
2.	GUO Xiang, ZHONG Cai Gao, ZHANG Yan Fang, LIU Fen, HE Jian, LIN Hui, GUO Mei Qiong. In Vitro Evaluation of Hemoperfusion for Chlorpyrifos Poisoning. Biomedical and Environmental Sciences. 2018(12): 922-926 . 必应学术

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文章访问数: 172
HTML全文浏览量: 13
PDF下载量: 19
被引次数: 2

气相色谱法测定血浆中毒死蜱及其主要代谢产物

作者简介: 郭翔(1982-),男,硕士,助理研究员、主管医师

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出版历程

Determination of chlorpyrifos and its metabolite in plasma by GC

期刊类型引用(2)

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目录

作者简介:
郭翔(1982-),男,硕士,助理研究员、主管医师