超高效液相色谱-串联质谱法测定泡泡液玩具中异噻唑啉酮类杀菌防腐剂  

Determination of Isothiazolinone Bactericides and Preservatives in Bubble Liquid Products by Ultra High Performance Liquid Chromatography-tandem Mass Spectrometry

作　　者：刘萍[1] 臧珊珊 LIU Ping;ZANG Shan-shan(College of Agriculture and Biotechnology,Taizhou Vocational College of Science&Technology,Taizhou 318020,China;Institute of Biophysics,Chinese Academy of Sciences,Beijing 100101,China)

机构地区：[1]台州科技职业学院农业与生物工程学院,浙江台州318020 [2]中国科学院生物物理研究所,北京100101

出　　处：《化学试剂》2020年第5期533-537,共5页Chemical Reagents

基　　金：2019年高等学校国内访问工程师“校企合作项目”(FG2019214)。

摘　　要：建立了超高效液相色谱-串联质谱(UPLC-MS/MS)同时测定泡泡液中2-甲基-4-异噻唑啉-3-酮(MI)、5-氯-2-甲基-4-异噻唑啉-3-酮(CMI)和1,2-苯并异噻唑啉-3-酮(BIT)含量的方法。考察了不同提取溶剂和提取时间对MI、CMI和BIT的提取结果的影响,以及不同流动相和不同色谱柱对MI、CMI和BIT的色谱分离效果。泡泡液样品经20%甲醇水溶液超声提取10 min,过滤膜后进样。以5 mmol/L乙酸铵水和5 mmol/L乙酸铵甲醇为流动相梯度洗脱,MI、CMI和BIT在C8柱上4.5 min内达到基线分离。MI、CMI和BIT分别在1~20、3~60和5~100μg/L范围内,相关系数r^2≥0.9992;信噪比法获得的MI、CMI和BIT定量限范围为0.06~0.1 mg/kg;MI、CMI和BIT在泡泡液阳性样品中3水平加标平均回收率范围为86.4%~108%,相对标准偏差范围为1.2%~4.5%。方法快速、简便、灵敏度高、重复性好、准确度高,定量限也满足欧盟指令中MI、CMI和BIT的限量要求,具有较好的实用性,并已用于实际样品的检测。An ultra high performance liquid chromatography-tandem mass spectrometry(UPLC-MS/MS)method was established to determine the contents of 2-methyl-4-isothiazolin-3-one(MI),5-chloro-2-methyl-4-isothiazolin-3-one(CMI)and 1,2-benzisothiazol 3-one(BIT)in bubble liquid products.The effects of different extraction solvents and extraction time were investigated,and different mobile phase components and chromatographic columns were also compared.The optimized sample pretreatment procedure was that the bubble liquid samples were extracted with 20%ethanol aqueous solution by sonification for 10 min,and then filtered with needle filters before injection.With 5 mmol/L ammonium acetate aqueous solution and 5 mmol/L ammonium acetate methanol solution as mobile phase and gradient elution,the base separations of MI、CMI and BIT could be achieved within 4.5 min on a C8 column.The correlation coefficient r^2 was greater than or equal 0.9992 in the range of 1~20,3~60,5~100μg/L.The limits of quantification(LOQs)were 0.06~0.1 mg/kg.The average recoveries for MI,CMI and BIT were 86.4%~108%with the relative standard deviation(RSD)1.2%~4.5%.The method is apt to operate and shows good accuracies and repeatabilities.The LOQs of MI、CMI and BIT are also met the requirements of relevant regulations.The method has been applied to analyze bubble liquid samples.

关 键 词：UPLC-MS/MS 泡泡液 异噻唑啉酮 杀菌 防腐剂 

分 类 号：O658[理学—分析化学]