Research on solid phase extraction and detection methods for tetrodotoxin in blood
10.13618/j.issn.1001-5728.2025.01.012
- VernacularTitle:血液中河豚毒素的固相萃取及检测方法研究
- Author:
Yu XUAN
1
;
Baofeng YANG
;
Si CHEN
;
Xiaocong ZHUO
;
Defeng FU
;
Jiancong SUN
Author Information
1. 浙江省公安厅刑侦总队 浙江省刑事科学技术应用研究重点实验室,浙江 杭州 310009
- Publication Type:Journal Article
- Keywords:
Blood;
Tetrodotoxin;
Solid phase extraction;
Liquid chromatography mass
- From:
Chinese Journal of Forensic Medicine
2025;40(1):65-69
- CountryChina
- Language:Chinese
-
Abstract:
Objective To establish a purification,enrichment and test method of tetrodotoxin in blood.Methods Through the investigation of various hydrophilic chromatographic columns,the comparison of extraction effects of different types of solid phase extraction columns and the interference analysis of mixed peaks on qualitative ion pairs,the matrix influence of tetrodotoxin was reduced,and the detection sensitivity and qualitative accuracy were improved.Results Tetrodotoxin is highly polar and easily inhibited by the matrix,while conventional precipitation protein method has low sensitivity and isomer double peaks,and the C18 column is not reserved.After comprehensive comparative analysis,the weak cation exchange column PWC column is finally used for purification and enrichment.Complete elution was achieved using 0.5 mL 10%formic acid and 50%acetonitrile aqueous solution.Seperation was performed on an Atlantis HILIC column,with qualitative ion pairs set at m/z,320.10>162.15 and 284.15.The detection limit of the method was 0.061 ng/mL.Conclusion The established PWC solid-phase extraction-LC/MS detection method demonstrates significant purification efficacy,minimal matrix influence,unobstructed chromatographic peaks,markedly improved detection sensitivity.This approach is operationally simple,and applicable to forensic casework.
