超高效液相色谱-串联质谱法测定鸡蛋中7种喹诺酮类药物的基质效应

研究了超高效液相色谱-串联质谱测定鸡蛋中7种喹诺酮类药物的基质效应。比较了鸡蛋中7种喹诺酮类药物经固相萃取柱净化法、正己烷除油法和未净化法3种前处理方法在高效液相色谱-串联质谱检测模式下基质效应的差异,结果表明固相萃取柱净化法方法优于其他两种,在此基础上进一步研究了不同称样量和目标化合物不同进样浓度的基质效应评价。结果表明随着称样量的增加,化合物的基质效应也越来越高;随着检测质量浓度的增大,目标化合物受基质效应的影响逐渐减小。因此在设计喹诺酮检测实验步骤时,首先应在保证方法灵敏度的前提下尽可能的减少称样量,其次可以采用固相萃取柱法作为净化步骤,能有效去除基质中大部分杂质,最后如果有合适的同位素内标物或者与化合物性质相似的物质,也可以用内标校正法来降低目标化合物的基质效应。

Matrix Effects in the analysis of seven Quinolones Residues in Eggs by UPLC-MS/MS

The matrix effect of seven quinolones in eggs was studied by ultra performance liquid chromatography tandem mass spectrometry(UPLC-MS/MS).In this paper,the matrix effects differences of seven quinolones in eggs were compared by three purification methods:solid phase extraction(SPE)purification method,n-hexane degreasing and unpurified meth?od.The results showed that the solid phase extraction(SPE)purification method was superior to the other two methods.On this basis,the matrix effect evaluation of different sample weighting and different injection concentration of the target com?pound was further studied.It was found that the matrix effect of the compounds increased with the increase of the sample weighting,and the influence of matrix effect on the target compounds decreased gradually with the increase of the detection concentration.Therefore,when designing the experimental procedure of quinolones,the author should first reduce the sam?ple weighting as much as possible on the premise of ensuring the sensitivity of the method,and then take solid phase extrac?tion(SPE)as the effectively purification step.Finally,if the appropriate isotope internal standard or the substance with sim?ilar properties can obtain,we can reduce the matrix effect of the target compound by internal standard method.