Simultaneous Determination of 21 Kinds of Aconitum Alkaloids in Biological Specimens and Herbal Wines Using Ultra-Performance Liquid Chromatography-Tandem Mass Spectrometry
10.19756/j.issn.0253-3820.251070
- VernacularTitle:超高效液相色谱-串联质谱法同时检测生物检材及泡酒中21种乌头类生物碱
- Author:
Ju YANG
1
;
Guo-Jun LI
;
Xian-Mou FAN
;
Rui-Bin ZHAO
;
Shao-Ming SU
;
Xu-Xian FU
;
En-Jin ZHU
;
Qi-Lin HUANG
;
Yao QIN
;
Li-Na LI
Author Information
1. 昆明医科大学法医学院,昆明 650500
- Keywords:
Aconitum alkaloids;
Ultra-high performance liquid chromatography-tandem mass spectrometry;
Forensic toxicology analysis;
Biological specimens
- From:
Chinese Journal of Analytical Chemistry
2025;53(8):1391-1401,后插1-后插6,封3
- CountryChina
- Language:Chinese
-
Abstract:
A method for simultaneous determination of 21 kinds of Aconitum alkaloids(ATS)in biological specimens and infused liquor using ultra-performance liquid chromatography-tandem mass spectrometry(UPLC-MS/MS)was developed.The biological samples were pretreated with methanol-acetonitrile(1∶2,V/V)for protein precipitation,while infused liquors were diluted 100-fold with acetonitrile,followed by centrifugation,and filtration by a 0.22-μm membrane.Chromatographic separation was carried out on an EC-C18 column using gradient elution with the mixture of 10 mmol/L ammonium acetate and 0.2%formic acid as mobile phase A and acetonitrile as mobile phase B.With this method,all the analytes were separated within 9.5 min.The samples were detected in positive ESI mode with dynamic multiple reaction monitoring(MRM)and quantified via external standard calibration.The results showed that the concentrations of the analytes in the range of 2-1000 ng/mL had excellent linearity(R2>0.9992)with the peak area.The developed method was successfully used for detection of 21 kinds of aconitum alkaloids,with limits of detection of 0.5-2 ng/mL,quantification limits of 2-6 ng/mL,intra/inter-day precision≤6.0%,spiked recoveries of 89.4%-100.9%,extraction recoveries of 74.2%-104.4%,and matrix effects ranging from-11.1%to 9.2%in blood/urine.The method was applied to detection of 12 samples from 4 fatal aconite poisoning cases,and all 21 kinds of ATS with total alkaloid concentrations of 0.04-4.18 μg/mL in blood and 154.96-422.83 μg/mL in medicinal liquors were detected.Tissue distribution revealed that the order of concentrations from highest to lowest is as follows:urine(157.22 μg/mL)>gastric contents(51.37 μg/mL)>kidney(21.6 μg/g)>whole blood(4.18 μg/mL)>liver(0.03 μg/g).This method showed many advantages such as simple pretreatment,low detection limits,accurate quantification,broad analyte coverage,and superior anti-interference capability in complex matrices,proving ideal for forensic and toxicological analysis of aconitum alkaloids.
