摘要
【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.
作者
孟冬玲
陈志燕
王维刚
朱文静
周芸
唐纲岭
杨飞
MENG Dongling;CHEN Zhiyan;WANG Weigang;ZHU Wenjing;ZHOU Yun;TANG Gangling;YANG Fei(China Tobacco Guangxi Industrial Co.,Ltd.,Nanning 530001;Guizhou Province Tobacco Quality Supervision Station,Guiyang 550025;China National Tobacco Quality Supervision&Test Center,Zhengzhou 450001)
出处
《中国烟草学报》
CAS
CSCD
北大核心
2022年第2期33-41,共9页
Acta Tabacaria Sinica
基金
中国烟草总公司标准制修订项目(2021QB016)。
关键词
烟用水基胶
超高效液相色谱-串联质谱
通过式固相萃取
异噻唑啉酮
烷基酚
烷基酚聚氧乙烯醚
alkylphenols
alkylphenol polyoxyethylene ethers
isothiazolinones
pass-through solid phase extraction
water-based adhesives
ultra performance liquid chromatography-tandem mass spectrometry
作者简介
孟冬玲(1975-),硕士,高级工程师,研究方向:样品前处理方法研究,Email:1694201009@qq.com;通讯作者:杨飞(1985-),硕士,高级工程师,研究方向:烟用材料检验方法研究,Email:Yangfei0797@163.com。
