Determination of Endosulfan Concentrations in Biological Samples by GC-MS/MS.
10.12116/j.issn.1004-5619.2018.04.007
- Author:
Fan ZHANG
1
;
Jun Yuan QIAO
2
;
Ming Jun YU
1
;
Juan JIA
1
;
Jie CAO
1
;
Chao ZHANG
1
;
Hai Yan CUI
1
;
Ke Ming YUN
1
;
Zhi Wen WEI
1
Author Information
1. School of Forensic Medicine, Shanxi Medical University, Taiyuan 030024, China.
2. Taiyuan Public Security Bureau, Taiyuan 030024, China.
- Publication Type:Journal Article
- Keywords:
biological samples;
endosulfan;
forensic toxicology;
gas chromatography-mass spectrometry;
poisoning
- MeSH:
Animals;
Chromatography, Gas/methods*;
Endosulfan/metabolism*;
Gas Chromatography-Mass Spectrometry/methods*;
Humans;
Limit of Detection;
Reproducibility of Results;
Tandem Mass Spectrometry/methods*
- From:
Journal of Forensic Medicine
2018;34(4):379-383
- CountryChina
- Language:English
-
Abstract:
OBJECTIVES:To establish an analytical method of the endosulfan concentrations （α-endosulfan and β-endosulfan） in biological samples by GC-MS/MS. To observe the distribution of endosulfan in aquatic animals and provide experimental evidence for forensic identification of relevant cases.
METHODS:Acetonitrile was added to the blood and muscle samples for precipitating the protein. The endosulfan concentrations were determined by GC-MS/MS in multiple reaction monitoring mode. Qualitative analysis was performed according to the retention time and ion rate, and quantitative analysis was performed by external standard working curve method.
RESULTS:In blood samples, the calibration curves of α-endosulfan and β-endosulfan ranging from 0.062 5 to 10 μg/mL had good linear relationship, the correlation coefficients （r） of which were >0.99. The limits of detection （LOD） were 1 ng/mL and 2 ng/mL and the limits of quantification （LOQ） were 4 ng/mL and 8 ng/mL, respectively. In muscle samples, the calibration curves of α-endosulfan and β-endosulfan ranging from 0.062 5 to 10 μg/g, the r of which were >0.98. The LOD were 1 ng/g and 4 ng/g and the LOQ were 4 ng/g and 16 ng/g, respectively. The accuracy of α-endosulfan and β-endosulfan was 90.76%-108.91% both in blood and muscle samples, the interday and intraday precision were 2.35%-8.71% and 5.44%-10.29%, respectively. In poisoning cases, endosulfan were detected in all parts of fish and crab and the content difference was statistically significant.
CONCLUSIONS:The endosulfan detection method based on GC-MS/MS established in the present study is rapid, sensitive and accurate, which can be applied to the endosulfan detection in traces biological samples. The distribution of endosulfan in fish and crab was different, which can provide evidence to the sample collection and analysis for toxicological analysis in relevant forensic identification.
