超高效液相色谱-串联质谱法测定烟用水基胶中14种杀菌剂  

Determination of 14 bactericides in water-based emulsion adhesives for cigarette by ultra performance liquid chromatography-tandem mass spectrometry

作　　者：夏志骋 钟杰 谢剑晨 黄灵洁 曹昌清 王颖[1] XIA Zhicheng;ZHONG Jie;XIE Jianchen;HUANG Lingjie;CAO Changqing;WANG Ying(Shanghai Provincial Tobacco Quality Inspection&Test Station,Shanghai 200082,China)

机构地区：[1]上海烟草集团有限责任公司质量监督检测站,上海200082

出　　处：《化学分析计量》2023年第7期35-41,共7页Chemical Analysis And Meterage

摘　　要：建立超高效液相色谱-串联质谱同时快速测定烟用水基胶中溴硝醇、尼泊金酯、山梨酸、苯甲酸及异噻唑啉酮的方法。烟用水基胶经水分散后,用甲醇萃取,离心后取上层清液过0.22μm有机滤膜,再稀释20倍后上机测定。选取ACQUITY BEH C_(18)(100 mm×2.1 mm,1.7μm)色谱柱,以水和甲醇为流动相分离,分别在电喷雾正负离子模式下和多反应监测(MRM)模式下检测。结果表明,所有待测物在各自的质量浓度范围内线性良好,相关系数均大于0.998,其中6种尼泊金酯(尼泊金甲酯、尼泊金乙酯、尼泊金丙酯、尼泊金异丙酯、尼泊金丁酯、尼泊金异丁酯)、5-氯-2-甲基-4-异噻唑啉-3-酮、2-正辛基-4-异噻唑啉-3-酮、4,5-二氯-N-辛基-4-异噻唑啉-3-酮的线性范围为0.25~10 ng/L;溴硝醇、2-甲基-4-异噻唑啉-3酮、1,2-苯并异噻唑-3-酮的线性范围为2.5~100 ng/L;山梨酸、苯甲酸的线性范围为25~1000 ng/L。线性相关系数均不小于0.998。方法的定量限为0.03~2.69μg/g。低、中、高3个浓度水平下,14种目标化合物在烟用水基胶中平均回收率为76.4%~125.4%,相对标准偏差为1.7%~12.2%(n=6)。该方法的精密度、准确度符合测定要求。该方法操作简单,准确灵敏,重复性好,适用于烟用水基胶中溴硝醇、尼泊金酯等杀菌剂的同时检测。A method was developed for the determination of bronopol,paraben,sorbic acid,benzoic acid and isothiazolone in water-based emulsion adhesives for cigarette by ultra performance liquid chromatography-tandem mass spectrometry(UPLC-MS/MS).The samples were dispersed in water and extracted by methanol.After centrifugation,the eluent was filtered through a 0.22μm organic filter membrane and diluted 20 times by methanol into an injection vial for detection by UPLC-MS/MS.The separation of target compounds was performed with Waters ACUQUITY BEH C_(18)(100 mm×2.1mm,1.7μm)by gradient elution,using water and methanol as the mobile phase.The analytes were detected with both positive ion electrospray ionization mode(ESI+)and negative ion electrospray ionization mode(ESI-)under the multiple reaction monitoring(MRM)mode.Under the optimal conditions,the parabens(methyl paraben,ethyl paraben,propyl paraben,isopropyl paraben,butyl paraben,isobutyl paraben),isothiazolone(5-chloro-2-methyl-4-isothiazolin-3-one,2-noctyl-4-isothiazolin-3-one,4,5-dichloro-2-n-octy-4-isothiazolin-3-one)were in the range of 0.25-10 ng/L;bronopol,2-methyl-4-isothiazolin-3-one,1,2-benzisothiazolin-3-one were in the range of 2.5-100 ng/L;sorbic acid and benzoic acid were in the range of 25-1000 ng/L,the correlation coefficients(r)were all not less than 0.998.The limits of quantitations were 0.03-2.69μg/g,the average recoveries at three spiked levels ranged from 76.4%-125.4%with relative standard deviations of 1.7%-12.2%(n=6).This method is simple,sensitive and accurate,and it is suitable for the determination of bactericide in water-based emulsion adhesives for cigarette.

关 键 词：超高效液相色谱-串联质谱法 烟用水基胶 溴硝醇 尼泊金酯 异噻唑啉酮 

分 类 号：O657.7[理学—分析化学]