超高效液相色谱-串联质谱法测定鸡蛋中15种药物残留

Simultaneous determination of 15 drugs residues in eggs by ultra performance liquid chromatography-tandem mass spectrometry

中文关键词:  固相萃取法  超高效液相色谱-串联质谱法  四环素  喹诺酮  鸡蛋  协方差分析

英文关键词:solid phase extraction  ultra performance liquid chromatography-tandem mass spectrometry  quinolones  tetracyclines  eggs  covariance analysis

中文摘要:

      目的 建立固相萃取-超高效液相色谱-串联质谱法(ultra performance liquid chromatography-tandem mass spectrometry, UPLC/MS/MS)测定鸡蛋中4种四环素类和11种喹诺酮类药物的同时分析方法。方法 通过实验设计与协方差分析, 找出检测方法的影响因素。样品经0.1 mol/L Mcllvaine-Na2EDTA缓冲液超声提取, 钨酸钠-硫酸溶液去蛋白, HLB固相萃取柱富集后用甲醇洗脱, 以超高效液相色谱-串联质谱仪多反应监测子模式, 基质匹配标准溶液定性、定量分析。结果 校准曲线在4~500 μg/L浓度范围内显示出良好的线性关系。15种药物相关系数r>0.995, 批内精密度为0.4%~5.3%, 方法检出限(S/N=3)为0.1~1.0 μg/kg, 方法检定量限(S/N=10)为0.3~3.0 μg/kg, 添加量为1.6、16.0和32.0 μg/kg的样品回收率为80.3%~110%。结论 本方法对样品前处理方法进行优化, 操作快速简单, 重复性好, 能对鸡蛋中四环素和喹诺酮类药物同时分析, 适合大量样品的定性和定量分析。

英文摘要:

      Objective To establish a method for simultaneous determination of 11 kinds of quinolones and 4 kinds of tetracyclines in eggs by solid phase extraction (SPE) and ultra performance liquid chromatography-tandem mass spectrometry (UPLC/MS/MS). Methods The positive cross experiment design and covariance analysis were used to find out the influencing factors of the detection method. Samples were ultrasound extracted by 0.1 mol/L Mcllvaine-Na2EDTA buffer, then deproteined using Na2WO4-H2SO4, and the extracts were subjected to HLB solid phase extraction(SPE) cartridges and eluted with methanol. A multiple reaction monitoring model was developed by ultra performance liquid chromatography tandem mass spectrometry, qualitative and quantitative analysis was carried out with matrix matching standard solution. Results The calibration curves showed good linearity within the concentrations of 4~500 μg/L with the correlation coefficients r of 15 kinds of drug above 0.995. The internal accuracy was 0.4%~5.3%, and the detection limit (S/N=3) of the method was 0.1~1.0 g/kg. The quantitative limit (S/N=10) of the method was 0.3~3.0 g/kg. The recoveries of 15 kinds of analytes were 80.3%~110% at the spiked levels of 1.6, 16.0 and 32.0 μg/kg. Conclusion The method is optimized for sample pretreatment, which is quick, simple and reproducible and can simultaneously analyze tetracycline and quinolones in eggs. It is suitable for the accurate qualitative and quantitative analysis of a large number of samples.