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固相萃取与超高效液相色谱/质谱联用同时测定动物源性食品中的琥珀胆碱及其代谢物。

Simultaneous determination of succinylcholine and its metabolite in animal-derived foods by solid-phase extraction combined with ultra-performance liquid chromatography/mass spectrometry.

机构信息

Department of Chemistry and Physics, Jilin Provincial Center for Disease Control and Prevention, Changchun, 130062, China.

出版信息

Rapid Commun Mass Spectrom. 2020 Oct 30;34(20):e8888. doi: 10.1002/rcm.8888.

Abstract

RATIONALE

Succinylcholine has been increasingly used in the theft of animals. Because of the presence of residual levels of succinylcholine in poisoned animals, it is harmful for people to eat foods derived from these animals. Therefore, a method should be immediately established to determine succinylcholine and its metabolite in animal-derived foods.

METHODS

A fast, highly sensitive method, combining solid-phase extraction (SPE) with ultra-performance liquid chromatography/electrospray ionization tandem mass spectrometry (UPLC/ESI-MS/MS), was developed for the determination of succinylcholine and its metabolite in animal-derived foods. The sample was initially extracted with heptafluorobutyric acid and then further cleaned up using an SPE cartridge. Succinylcholine and its metabolite were separated using acetonitrile: 0.1% formic acid in 5 mmol L ammonium acetate as the mobile phase. Quantitative results were based on positive ion ESI multiple reaction monitoring mode.

RESULTS

The results show good linearity over a wide range with correlation coefficients of determination of more than 0.998. Both the limits of detection of succinylcholine and succinylmonocholine are 0.2 μg kg . The intra- and inter-day accuracies of the method are in the range 91.4%-104.6%, and the intra- and inter-day precisions are in the range 2.5%-6.6%.

CONCLUSIONS

This method can be used for the determination of succinylcholine as an illicit drug in animal-derived foods. It was successfully applied to the identification and quantification of succinylcholine and succinylmonocholine in animal-derived foods collected from a local farmers market in Jilin Province of China.

摘要

原理

越来越多的人在偷动物时使用琥珀酰胆碱。由于中毒动物体内仍存在琥珀酰胆碱残留水平,因此人们食用这些动物来源的食物是有害的。因此,应立即建立一种方法来确定动物源性食品中的琥珀酰胆碱及其代谢物。

方法

建立了一种快速、灵敏的方法,结合固相萃取(SPE)和超高效液相色谱/电喷雾串联质谱(UPLC/ESI-MS/MS),用于测定动物源性食品中的琥珀酰胆碱及其代谢物。样品先用庚氟丁酸提取,然后用 SPE 小柱进一步净化。采用乙腈:0.1%甲酸在 5mmol/L 乙酸铵中的溶液作为流动相分离琥珀酰胆碱及其代谢物。定量结果基于正离子 ESI 多反应监测模式。

结果

结果表明,在很宽的范围内具有良好的线性关系,决定系数均大于 0.998。琥珀酰胆碱和琥珀酰单胆碱的检测限均为 0.2μg/kg。该方法的日内和日间准确度在 91.4%-104.6%之间,日内和日间精密度在 2.5%-6.6%之间。

结论

该方法可用于检测动物源性食品中的非法药物琥珀酰胆碱。成功应用于中国吉林省当地农贸市场采集的动物源性食品中琥珀酰胆碱和琥珀酰单胆碱的鉴定和定量。

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