通过式固相萃取结合UPLC-MS/MS同时测定烟用水基胶中的烷基酚、烷基酚聚氧乙烯醚和异噻唑啉酮

Simultaneous determination of alkylphenols, alkylphenol polyoxyethylene ethers and isothiazolinones in water-based adhesives of cigarette by ultra performance liquid chromatography-tandem mass spectrometry combined with pass-through SPE

【目的】建立通过式固相萃取结合超高效液相色谱-串联质谱(UPLC-MS/MS)同时测定烟用水基胶中烷基酚、烷基酚聚氧乙烯醚和异噻唑啉酮杀菌剂的方法。【方法】样品用甲醇提取,经PRi ME HLB通过式固相萃取净化后,以ACQUITY UPLC HSS C18 SB (100 mm×3.0 mm, 1.8μm)为色谱柱,水和甲醇为流动相进行梯度洗脱。【结果】所有分析物回收率在86.6%~104.4%之间,日内精密度为1.5%~5.6%,日间精密度为2.3%~5.1%。在8~800ng/m L的浓度范围内所有化合物均有良好的线性关系(r^(2)≥0.9991),检出限(LOD)和定量限(LOQ)范围分别为0.17~0.62mg/kg和0.54~1.94 mg/kg。【结论】该方法快速、准确、选择性强,可用于烟用水基胶样品中烷基酚、烷基酚聚氧乙烯醚和异噻唑啉酮杀菌剂的同时测定。

[Objective] To realize the determination of alkylphenols, alkylphenol ethoxylatesand isothiazolinones in water-based adhesives of cigarette, ultra performance liquid chromatography-tandem mass spectrometry(UPLC-MS/MS) analytical method combined with pass-through solid phase extraction was established. [Methods] The sample was extracted with methanol and purified by a PRiME HLB pass-through solid-phase extraction, followed by separation treatment with ACQUITY UPLC HSS C18 SB(100 mm×3.0 mm, 1.8 μm)chromatographic column using water and methanol as mobile phases. [Results] The results showed that: within 12 minutes, all analytes were eluted;under optimized conditions, the recoveries for all compounds were 80.8%-95.5%, with relative standard deviations(RSDs)less than 7.0%. Good coefficients of determination(R^(2)≥0.9991) were achieved for all studied analytes. The LOD for all analytes varied from 0.17-0.62 mg/kg and the LOQ varied from 0.54-1.94 mg/kg. [Conclusion] The results confirm that the proposed method is stable and reliable, and can be used to determine alkylphenols, alkylphenol polyoxyethylene ethers and isothiazolinones in water-based adhesives of cigarette.