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J Chromatogr B Analyt Technol Biomed Life Sci. 2016 Aug 1;1027:96-102. doi: 10.1016/j.jchromb.2016.05.030. Epub 2016 May 24.

Optimized ultra performance liquid chromatography tandem high resolution mass spectrometry method for the quantification of paraquat in plasma and urine.

Author information

1
Department of Hygienic Analysis and Detection, Key Lab of Modern Toxicology, Ministry of Education, School of Public Health, Nanjing Medical University, 818 Tianyuan East Road, Nanjing, 211166, China.
2
Department of Emergency Medicine, The First Affiliated Hospital of Nanjing Medical University, 300 Guangzhou Road, Nanjing, 210029, China.
3
Department of Toxicology, Key Lab of Modern Toxicology, Ministry of Education, School of Public Health, Nanjing Medical University, 818 Tianyuan East Road, Nanjing, 211166, China.
4
Department of Hygienic Analysis and Detection, Key Lab of Modern Toxicology, Ministry of Education, School of Public Health, Nanjing Medical University, 818 Tianyuan East Road, Nanjing, 211166, China. Electronic address: gaorong@njmu.edu.cn.

Abstract

A simple, sensitive and specific ultra performance liquid chromatography coupled to electrospray tandem high resolution mass spectrometry (UPLC-ESI-HRMS/MS) method has been developed and validated for quantification of paraquat in plasma and urine. The sample preparation was carried out by one-step protein precipitation with acetonitrile. The paraquat was separated with a HILIC column in 10min. Detection was performed using Q Exactive Orbitrap mass spectrometer by Targeted-MS/MS scan mode. Methodological parameters, such as ammonium formate concentration, formic acid concentration, spray voltage, capillary temperature, heater temperature and normalized collision energy were optimized to achieve the highest sensitivity. The calibration curve was linear over the concentration range of LOQ-1000ng/mL. LOD was 0.1 and 0.3ng/mL, LOQ was 0.3 and 0.8ng/mL for urine and plasma, respectively. The intra- and inter-day precisions were <7.97% and 4.78% for plasma and urine. The accuracies were within the range 93.51-100.90%. The plasma and urine matrices had negligible relative matrix effect in this study. This method was successfully applied to determine paraquat concentration in plasma samples with hemoperfusion from 5 suspected paraquat poisoning patients.

KEYWORDS:

HILIC column; Paraquat; Plasma; UPLC-ESI-HRMS/MS; Urine

PMID:
27270261
DOI:
10.1016/j.jchromb.2016.05.030
[Indexed for MEDLINE]

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