[1]丁婕,何宇敏,王晓萍.血浆中有机磷液相色谱-质谱法测定方法的建立[J].福建医药杂志,2022,44(04):117-120.
　DING Jie,HE Yumin,WANG Xiaoping.Establishment of a liquid chromatography/mass spectrometry method for detecting the plasma concentration of organophosphorus[J].FUJIAN MEDICAL JOURNAL,2022,44(04):117-120.
点击复制

血浆中有机磷液相色谱-质谱法测定方法的建立()
分享到：

《福建医药杂志》[ISSN:1002-2600/CN:35-1071/R]

卷:
44
期数:
2022年04期
页码:
117-120
栏目:
基础研究
出版日期:
2022-08-15

文章信息/Info

Title:
Establishment of a liquid chromatography/mass spectrometry method for detecting the plasma concentration of organophosphorus
文章编号:
1002-2600(2022)04-0117-04
作者:
丁婕; 何宇敏; 王晓萍1
福建医科大学省立临床医学院 福建省立医院急诊科 福建省急诊医学重点实验室（福州 350001）
Author(s):
DING Jie;  HE Yumin;  WANG Xiaoping
Fujian Provincial Key Laboratory of Emergency Medicine;Department of Emergency Medicine, Fujian Provincial Hospital;Shengli Clinical Medical College of Fujian Medical University, Fuzhou, Fujian 350001, China
关键词:
液相色谱-质谱法; 有机磷; 定量检测
Keywords:
liquid chromatography/mass spectrometry;  organophosphorus;  quantitative detection
分类号:
R.331
文献标志码:
A
摘要:
目的 建立液相色谱-质谱法（liquid chromatography/mass spectrometry，LC/MS）测定血浆中氧化乐果、敌敌畏、克百威、乐果浓度的方法。方法 使用纯乙腈沉淀蛋白提取样品后，利用LC/MS法对提取的样品进行检测。对建立方法的线性、精密度、加标回收率进行评价。结果 氧化乐果在10~200 ng/mL、100~1 000 ng/mL的浓度范围内线性关系良好，最低定量限为10 ng/mL；敌敌畏、克百威、乐果在50~1 000 ng/mL、1 000~5 000 ng/mL的浓度范围内线性关系良好，最低定量限均为50 ng/mL；氧化乐果、敌敌畏、克百威、乐果的批内精密度均在±10%范围内，批间精密度在±15%范围内氧化乐果的回收率在92.89%~98.35%，敌敌畏的回收率为94.36%~98.27%，克百威的回收率为92.74%~97.28%，乐果的回收率为90.36%~96.48%。结论 建立的LC/MS方法可用于血浆中有机磷的定性和定量检测。
Abstract:
Objective To establish a liquid chromatography/mass spectrometry (LC/MS) method for detecting the plasma concentration of organophosphorus．Methods The samples were extracted by acetonitrile,and the extracted samples were detected by LC/MS．The linear of the method, precision and standard recovery rate were evaluated．Results The relationship between the sample concentration and the peak area of mass spectrum response was linear within 10~200 ng/mL,100~1 000 ng/mL in omethoate，and the minimum limit of quantitation was 10 ng/mL；The relationship between the sample concentration and the peak area of mass spectrum response was linear within 50~1 000 ng/mL,1 000~5 000 ng/mL in dichlorvos, carbofuran, dimethoate,and the minimum limit of quantitation was 50 ng/mL.The intraassay precision of omethoate, dichlorvos, carbofuran and dimethoate was within ±10%, and the inter-assay precision was within ±15%．The recovery rate of omethoate, dichlorvos, carbofuran, dimethoate were 92.89%~98.35%, 94.36%~98.27%, 92.74%~97.28%, 90.36%~96.48% respectively. Conclusion The LC/MS method we established can be used for the qualitative and quantitative detection of omethoate, dichlorvos, carbofuran and dimethoate in plasma.

参考文献/References:

[1] 杨立山,卢中秋,田英平．急性有机磷农药中毒诊治临床专家共识(2016)[J]．中国急救医学，2016,36(12):1057-1065.
[2] 张在其,梁仁,黄韬,等.全血、血浆、红细胞胆碱酯酶活性在急性有机磷农药中毒病程中的变化及意义[J]．中华急诊医学杂志,2001,10(4):232-234.
[3] 杨立山,李文峰,马晓,等．血液灌流对急性有机磷农药中毒血胆碱酯酶活力恢复的影响研究[J]．宁夏医学杂志,2011,33(6)：509-511.
[4] 王新平,曹国辉.血药浓度监测在急性有机磷农药中毒救治中的作用[J]．山东医药,2010,50(9):96.
[5] 何宇敏，柯俊，章九云,等. 血浆中百草枯、敌草快液相色谱-质谱法测定方法建立[J]．创伤与急诊电子杂志，2020,8,(3): 111-117.
[6] 中华医学会检验医学分会. 液相色谱-质谱临床应用建议[J]．中华检验医学杂志, 2018, 40(10): 770-779.
[7] 李小娟，何颖霞，朱宝立, 等. 人血清中有机磷农药QuEChERS法提取的气相色谱-质谱联用法测定[J]．中华劳动卫生职业病杂志,2018,36(5):378-381.
[8] 董芳,李惠玲,马婧.全血中有机磷农药和鼠药测定的QuEChERS前处理法[J]．中华劳动卫生职业病杂志,2016,34(10):782-785.
[9] 林抗美,马丽娜,朱育菁,等. 乐果液相色谱与气相色谱检测方法比较[J]．中国农学通报,2008,24(10):453-456.
[10] 林静.质谱联用技术及其在临床上的应用[J]．医学综述,2010,16(4):628-631.
[11] 李鹏,柏泽新,夏侯秋锦,等. UPLC-MS/MS检测人血中18忠有机磷及氨基酸酯类农药[J]．中国法医学杂志,2017,32(1):51-54.
[12] 王贤亲,林丹．LC-MS/MS测定人血浆5种有机磷的含量[J]．中国卫生检验杂志,2008,18(12):2537-2539.
[13] Inoue S, Saito T, Mase H. Rapid simultaneous determination fore organophosphorus pesticides in human serum by LC-MS[J]．Journal of Pharmaceutical and Biomedical Analysis, 2007, 44: 258-264.
[14] 黄宝勇,肖志勇,欧阳喜辉. 不同贮存条件对蔬菜基质中13种农药残留稳定性的影响[J]．农药科学与管理, 2013(2):29-34.
[15] 闵涛, 刘永涛, 徐子振,等. 常见有机磷农药稳定性研究进展[J]．毒理学杂志,2018,32(2): 164-167.

备注/Memo

备注/Memo:
基金项目：福建省自然科学基金项目（青年创新）（2020J05263）
1 通信作者
更新日期/Last Update: 2022-08-15