超高效液相色谱-四极杆飞行时间质谱法测定狗肉中的氯化琥珀胆碱

Determination of Succinylcholine Chloride in Dog Meat by UPLC-Q-TOF/MS

目的:建立固相萃取净化结合UPLC-Q-TOF/MS法测定狗肉中的氯化琥珀胆碱的分析方法。方法:样品经30%乙腈水提取后,氨水调节pH值至9.0,使用WCX固相萃取柱净化,电喷雾电离源(Electrospray Ionization,ESI)正模式进行电离。结果:氯化琥珀胆碱的基质曲线在1.0~100.0μg·L^(-1)线性较好,相关系数r^(2)为0.9992,方法的检出限和定量限分别为10μg·kg^(-1)和30μg·kg^(-1)。不同水平的平均回收率在86.3%~91.6%,相对标准偏差为2.99%~5.54%。结论:方法回收率高,重现性好,可准确测定狗肉中的氯化琥珀胆碱含量,并排除假阳性情况。

Objective:An analytical method was established for the determination of succinylcholine chloride in dog meat by solid phase extraction purification combined with ultra performance liquid chromatography-quadrupole time-of-flight mass spectrometry.Method:After the sample was extracted with 30%acetonitrile water,the pH was adjusted to 9.0 by ammonia,then the WCX solid phase extraction column was used for purification and finally the electrospray ionization source(Electrospray Ionization,ESI)positive mode was used for ionization.Result:The matrix curve of succinylcholine chloride was within the concentration of 1.0~100.0μg·L^(-1) and the linearity was good with the correlation coefficient r^(2)(0.9992).The limit of detection and limit of quantification were 10μg·kg^(-1) and 30μg·kg^(-1),respectively.The average recovery rate of different spiked levels was 86.3%~91.6%while the relative standard deviation(RSD)was 2.99%~5.54%.Conclusion:The method had high recovery rate and good reproducibility that could accurately determine the content of succinylcholine in dog meat and eliminate false positives.