高效液相色谱-串联质谱法测定烟用香精香料中的甲基异噻唑啉酮及其氯代物的含量

HPLC-MS/MS Determination of Methyl Isothiazolin Ketone and Its Chloro-Derivatives in Perfume and Essential Additives of Tobacco

采用高效液相色谱-串联质谱法测定烟用香精香料中的甲基异噻唑啉酮及其氯代物的含量。样品采用甲醇提取,以Agilent ZORBAX 300SB-C8色谱柱为分离柱,以不同体积比的甲醇和水混合液为流动相进行梯度洗脱,采用电喷雾正离子源多反应监测模式检测。甲基异噻唑啉酮及其氯代物的线性范围均为0.05~5.0mg·L^(-1),检出限分别为3.2,3.6μg·L^(-1)。加标回收率在77.1%~95.0%之间,测定值的相对标准偏差(n=6)均不大于5.0%。

HPLC-MS/MS was applied to the determination of methyl isothiazolin ketone and its chloroderivatives in perfume and essential additives of tobacco.The sample was extracted with methanol,and the extract was separated on Agilent ZORBAX 300SB-C8 column,using mixtures of methanol and water（mixed in different ratios）as mobile phase in gradient elution.ESI＋and multi-reaction monitoring mode were adopted in MS/MS determination.Linearity ranges of methyl isothiazolin ketone and its chloro-derivatives were found same between0.05mg·L^（-1） and 5.0mg·L^（-1）,with detection limits of 3.2,3.6μg·L^（-1） respectively.Values of recovery found by standard addition method were in the range of 77.1%-95.0%,and values of RSD′s（n=6）no more than 5.0%.