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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-Na_2EDTA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4~500μg/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0.1~1.0μg/kg,方法检定量限(S/N=10)为0.3~3.0μg/kg,添加量为1.6、16.0和32.0μg/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。
Objective To establish a simultaneous method for the determination of four tetracyclines and eleven quinolones in eggs by ultra performance liquid chromatography-tandem mass spectrometry (UPLC / MS / MS). Methods Through experimental design and analysis of covariance, find out the influencing factors of detection methods. The samples were extracted by 0.1 mol / L Mcllvaine-Na2EDTA buffer solution, deproteinized by sodium tungstate-sulfuric acid solution and enriched by HLB solid-phase extraction. The samples were eluted with methanol and analyzed by ultra performance liquid chromatography-tandem mass spectrometry Mode, matrix matching standard solution qualitative and quantitative analysis. Results The calibration curve showed a good linearity in the range of 4 ~ 500μg / L. The correlation coefficients of the 15 drugs were> 0.995. The intra-assay precision was 0.4% -5.3%. The detection limit (S / N = 3) was 0.1-1.0 μg / 0.3 ~ 3.0μg / kg, the recoveries of samples of 1.6, 16.0 and 32.0μg / kg were 80.3% ~ 110%. Conclusion The method of sample pretreatment optimization, fast and simple operation, good repeatability, tetracycline and quinolones in eggs can be simultaneously analyzed for a large number of samples qualitative and quantitative analysis.