UPLC-MS/MS法监测污水中甲卡西酮稳定性试验研究

Stability test study for monitoring methcathinone in sewage based on a UPLC-MS/MS method

目的通过正交试验比较甲卡西酮在不同溶剂pH值、浓缩温度、保存时间和保存温度提取条件下的稳定性,建立适合污水中甲卡西酮稳定测定的提取制备方法用于超高压液相色谱质谱联用仪的检测。方法在甲卡西酮检测过程中设置4个因素(提取溶剂pH值、浓缩温度、保存时间、保存温度)进行考察,每个因素选择3个水平,然后采用L9(34)进行正交试验,提取液使用液相色谱三重四极杆串联质谱仪(Exion LC/QTRAP 6500)检测,以甲卡西酮m/z=105.1的子离子峰面积作为定量指标,采用SPSS 16.0统计软件进行数据分析找出最佳条件。结果正交试验结果分析表明,提取溶剂pH=2.0,保存时间0d,保存温度-20℃,浓缩温度60℃为最佳提取条件,并根据该条件进行了方法学考察,结果表明甲卡西酮在1ng/L~500ng/L浓度范围内线性良好,提取回收率>90%,RSD<5.33%,基质效应<6.52%,RSD<0.31%,均符合相关标准要求。结论本研究通过正交试验筛选到的甲卡西酮制备方法有利于其稳定检测,适用于质谱的定性定量分析,可用于对污水中甲卡西酮成分的监测工作。

Objective Orthogonal tests were conducted to compare the stability of methcathinone under different extraction conditions including solvent p H, concentration temperature, storage time and storage temperature. An extraction and preparation method suitable for stable determination of methcathinone by ultra-high pressure liquid chromatography was established. Methods Four factors(extraction solvent pH value, concentration temperature, storage time, storage temperature) were observed, and three levels was chosen for each factor in the L9(34) orthogonal experiment. The extracts were detected by liquid chromatography coupled with triple quadrupole tandem mass spectrometry(Exion LC/QTRAP 6500), and the peak area of the sub ion with m/z=105.1 was used as the quantitative index. SPSS 16.0 statistical software was used to analyze the data to find the optimal conditions. Results Orthogonal test results showed that the optimal extraction conditions were: extraction solvent pH 2.0, storage time 0 day, storage temperature-20℃ and concentration temperature 60℃. Methodological investigation was carried out according to these conditions. The results showed that the concentration of methcathinone was linear in the range of 1 ng/L ~ 500 ng/L. The extraction recovery was more than 90%, RSD was less than 5.33%, matrix effect was less than 6.52% and RSD was less than 0.31%.All met the requirements of relevant standards. Conclusion The preparation method of methcathinone established by the orthogonal test in this study is conducive to stable detection and suitable for qualitative and quantitative analysis by mass spectrometry, and can be used for monitoring the level of methcathinone in sewage.