• 文献检索
  • 文档翻译
  • 深度研究
  • 学术资讯
  • Suppr Zotero 插件Zotero 插件
  • 邀请有礼
  • 套餐&价格
  • 历史记录
应用&插件
Suppr Zotero 插件Zotero 插件浏览器插件Mac 客户端Windows 客户端微信小程序
定价
高级版会员购买积分包购买API积分包
服务
文献检索文档翻译深度研究API 文档MCP 服务
关于我们
关于 Suppr公司介绍联系我们用户协议隐私条款
关注我们

Suppr 超能文献

核心技术专利:CN118964589B侵权必究
粤ICP备2023148730 号-1Suppr @ 2026

文献检索

告别复杂PubMed语法,用中文像聊天一样搜索,搜遍4000万医学文献。AI智能推荐,让科研检索更轻松。

立即免费搜索

文件翻译

保留排版,准确专业,支持PDF/Word/PPT等文件格式,支持 12+语言互译。

免费翻译文档

深度研究

AI帮你快速写综述,25分钟生成高质量综述,智能提取关键信息,辅助科研写作。

立即免费体验

采用干基质点取样和 GC-MS/MS 分析方法测定血液中的有机磷杀虫剂。

New analytical approach to determine organophosphorus insecticides in blood by dried matrix spots sampling and GC-MS/MS.

机构信息

Centro de Investigação em Ciências da Saúde (CICS-UBI), Universidade da Beira Interior, Av. Infante D. Henrique, 6201-556, Covilhã, Portugal.

Laboratório de Fármaco-Toxicologia, UBIMedical, Universidade da Beira Interior, Convento de Sto. António, 6201-001, Covilhã, Portugal.

出版信息

Anal Bioanal Chem. 2018 Dec;410(30):7955-7964. doi: 10.1007/s00216-018-1417-8. Epub 2018 Nov 7.

DOI:10.1007/s00216-018-1417-8
PMID:30402676
Abstract

This work describes the optimization of a new method for the determination of five organophosphorus insecticides in whole blood. The analytes were extracted from the matrix (50 μL) using the dried blood spot (DBS) approach and were analyzed by gas chromatography (GC) coupled to tandem mass spectrometry (MS/MS). The studied compounds (diazinon, chlorpyrifos, parathion-ethyl, chlorfenvinphos and quinalphos) were chosen based on the statistics of intoxications in Portugal, and ethion was used as internal standard. The method was fully validated, taking into account international guidelines for bioanalytical method validation, such as those of the Food and Drug Administration (FDA), International Conference on Harmonization (ICH) and Scientific Working Group for Forensic Toxicology (SWGTOX). A linear range of 0.1-25 μg/mL was obtained for all compounds, except for diazinon and quinalphos (0.05-25 μg/mL and 0.25-25 μg/mL, respectively), presenting determination coefficients above 0.99. Concerning precision, the coefficients of variation (CVs) were lower than 14% for all compounds. Those compounds were found to be stable in the samples. Although the values obtained for recovery were low (between 1 and 12%), the method proved to be sensitive, since detection limits between 0.05 and 0.1 μg/mL were obtained. The novelty is the use of the DBS approach in the extraction of these compounds, and this is the first paper reporting it: DBS is a recent technique of bioanalysis in the field of toxicology, and in addition to its simplicity and sensitivity, it is applicable routinely in both clinical and forensic toxicology situations. Graphical abstract ᅟ.

摘要

这项工作描述了一种新方法测定全血中五种有机磷杀虫剂的优化。采用干血斑(DBS)法从基质(50μL)中提取分析物,并用气相色谱(GC)串联质谱(MS/MS)进行分析。选择研究化合物(二嗪农、毒死蜱、乙基对硫磷、氯芬磷和喹硫磷)是基于葡萄牙中毒统计数据,并用乙硫磷作为内标。该方法是完全验证的,考虑到生物分析方法验证的国际指南,如美国食品和药物管理局(FDA)、国际协调会议(ICH)和法医毒理学科学工作组(SWGTOX)的指南。除二嗪农和喹硫磷(0.05-25μg/mL 和 0.25-25μg/mL)外,所有化合物的线性范围均为 0.1-25μg/mL,测定系数均大于 0.99。关于精密度,所有化合物的变异系数(CVs)均低于 14%。这些化合物在样品中稳定。虽然回收率值较低(在 1%到 12%之间),但该方法证明是敏感的,因为检测限在 0.05 到 0.1μg/mL 之间。新颖之处在于采用 DBS 法提取这些化合物,这是首次报道:DBS 是毒理学领域生物分析的一项新技术,除了简单和敏感之外,它还适用于临床和法医毒理学情况的常规应用。

相似文献

1
New analytical approach to determine organophosphorus insecticides in blood by dried matrix spots sampling and GC-MS/MS.采用干基质点取样和 GC-MS/MS 分析方法测定血液中的有机磷杀虫剂。
Anal Bioanal Chem. 2018 Dec;410(30):7955-7964. doi: 10.1007/s00216-018-1417-8. Epub 2018 Nov 7.
2
Determination of eight selected organophosphorus insecticides in postmortem blood samples using solid-phase extraction and gas chromatography/mass spectrometry.采用固相萃取和气相色谱/质谱法测定死后血样中的八种有机磷杀虫剂。
Rapid Commun Mass Spectrom. 2010 Nov 15;24(21):3187-94. doi: 10.1002/rcm.4765.
3
Determination of antipsychotic drugs in oral fluid using dried saliva spots by gas chromatography-tandem mass spectrometry.采用气相色谱-串联质谱法测定唾液干斑中的抗精神病药物。
Anal Bioanal Chem. 2019 Sep;411(23):6141-6153. doi: 10.1007/s00216-019-02005-8. Epub 2019 Jul 10.
4
Analysis of organophosphorus pesticides in whole blood by GC-MS-μECD with forensic purposes.采用气相色谱-质谱联用-微池电子捕获检测器对全血中的有机磷农药进行法医用途分析。
J Forensic Leg Med. 2015 Jul;33:28-34. doi: 10.1016/j.jflm.2015.03.006. Epub 2015 Mar 28.
5
Dried blood spots as a sampling technique for the quantitative determination of guanfacine in clinical studies.干血斑作为临床研究中胍法辛定量测定的一种采样技术。
Bioanalysis. 2011 Nov;3(22):2501-14. doi: 10.4155/bio.11.262.
6
Microwave-assisted on-spot derivatization for gas chromatography-mass spectrometry based determination of polar low molecular weight compounds in dried blood spots.基于气相色谱-质谱联用的微波辅助现场衍生化法测定干血斑中的极性低分子量化合物
J Chromatogr A. 2016 Sep 23;1465:175-83. doi: 10.1016/j.chroma.2016.08.057. Epub 2016 Aug 26.
7
Fully automated determination of nicotine and its major metabolites in whole blood by means of a DBS online-SPE LC-HR-MS/MS approach for sports drug testing.采用干血斑在线固相萃取液相色谱-高分辨串联质谱法全自动测定全血中的尼古丁及其主要代谢物用于运动药物检测。
J Pharm Biomed Anal. 2016 May 10;123:132-40. doi: 10.1016/j.jpba.2016.02.009. Epub 2016 Feb 10.
8
Validation of a dried blood spot LC-MS/MS approach for cyclosporin A in cat blood: comparison with a classical sample preparation.建立猫血液中环孢素 A 的干血斑 LC-MS/MS 检测方法的验证:与经典样品前处理方法的比较。
J Pharm Biomed Anal. 2012 Jul;66:298-305. doi: 10.1016/j.jpba.2012.03.049. Epub 2012 Apr 2.
9
Simultaneous determination of organophosphorus pesticides and phthalates in baby food samples by ultrasound-vortex-assisted liquid-liquid microextraction and GC-IT/MS.超声涡旋辅助液液微萃取-气相色谱-离子阱串联质谱法同时测定婴儿食品中的有机磷农药和邻苯二甲酸酯
Anal Bioanal Chem. 2018 May;410(14):3285-3296. doi: 10.1007/s00216-018-0986-x. Epub 2018 Mar 17.
10
Dried blood spots combined to an UPLC-MS/MS method for the simultaneous determination of drugs of abuse in forensic toxicology.干血斑结合 UPLC-MS/MS 法用于法医毒理学中滥用药物的同时测定。
J Pharm Biomed Anal. 2018 Jan 5;147:634-644. doi: 10.1016/j.jpba.2017.02.046. Epub 2017 Feb 27.

引用本文的文献

1
Interpol review of toxicology 2016-2019.国际刑警组织2016 - 2019年毒理学综述
Forensic Sci Int Synerg. 2020 May 23;2:563-607. doi: 10.1016/j.fsisyn.2020.01.018. eCollection 2020.
2
Experimental central composite design-based dispersive liquid-liquid microextraction for HPLC-DAD determination of diazinon in human urine samples: method development and validation.基于实验中心组合设计的分散液相微萃取-高效液相色谱-二极管阵列检测法测定人尿液中的敌敌畏:方法开发与验证。
Arh Hig Rada Toksikol. 2020 Mar 1;71(1):48-55. doi: 10.2478/aiht-2020-71-3292.
3
Organophosphorus pesticide determination in biological specimens: bioanalytical and toxicological aspects.
生物标本中有机磷农药的测定:生物分析和毒理学方面。
Int J Legal Med. 2019 Nov;133(6):1763-1784. doi: 10.1007/s00414-019-02119-9. Epub 2019 Jul 12.