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《化学分析计量》 2018年第02期
DOI:10.3969/j.issn.1008-6145.2018.02.003
超高效液相色谱-串联质谱法测定湿巾中 5种异噻唑啉酮类防腐剂
姚帮本,包磊,韩枫,郭佳佳
安徽省产品质量监督检验研究院,合肥 230051 
Determination of 5 isothiazolinone preservatives in wet wipes by ultra-performance liquid chromatography-tandem mass spectrometry
YAO Bangben, BAO Lei, HAN Feng, GUO Jiajia
Anhui Province Product Quality Supervision and Inspection Institute, Hefei 230051, China 
摘要:建立超高效液相色谱-串联质谱法快速测定湿巾中2-甲基-4-异噻唑啉-3-酮、5-氯-2-甲基-4-异噻唑啉-3-酮、1,2-苯并异噻唑啉-3-酮、2-正辛基-4-异噻唑啉-3-酮和4,5-二氯-2-正辛基-4-异噻唑啉-3-酮5种异噻唑啉酮类防腐剂的含量。样品经甲醇超声提取后用超高效液相色谱-串联质谱法测定。以甲醇-水为流动相,梯度洗脱,在多反应监测(MRM)模式下定性,外标法定量。5种异噻唑啉酮的质量浓度在1.0~100.0 μg/L范围内与色谱峰面积均呈良好的线性关系,r≥0.9995,方法定量限均为0.005 mg/kg。平均加标回收率为91.1%~103.5%,测定结果的相对标准偏差为2.11%~3.27%(n=6)。该方法样品前处理简单,检测灵敏度高,能快速测定湿巾中异噻唑啉酮的含量。 
Abstract:A method for simultaneous determination of 5 isothiazolinone preservatives such as 2-methyl-4-isothiazolin-3-one, 5-chloro-2-methyl-4-isothiazolin-3-one, 1,2-benzylisothiazolin-3-one, 2-octyl-4-isothiazolin-3-one and 4,5-dichloro-2-octyl-4-isothiazolin-3-one in wet wipes based by ultra-performance liquid chromatography-tandem mass spectrometry(UPLC-MS/MS) was developed. After ultrasonic extraction with methanol, the isothiazolinones were separated using methanol-water as mobile phases under gradient elution, then analyzed by UPLC-MS/MS in multiple reaction monitoring (MRM) mode. The concentration of isothiazolinone was linear with chromatographic area in the range of 1.0-100.0 μg/L. The correlation coefficients were not less than 0.9995, and the quantification limits were 0.005 mg/kg. The recoveries of the 5 isothiazolinones in wet wipes were in the range of 91.1%-103.5%, the relative standard deviations of detection results were 2.11%-3.27%(n=6). This method is simple in sample pretreatment, has high sensitivity, it is suitable for the quick determination of isothiazolinone antibacterial agents in wet wipes. 
关键词:异噻唑啉酮;超高效液相色谱-串联质谱法;湿巾;防腐剂 
Keywords:isothiazolinone; ultra-performance liquid chromatography-tandem mass spectrometry; wet wipes; preservative 
本文引用格式:
姚帮本,包磊,韩枫,等.超高效液相色谱-串联质谱法测定湿巾中5种异噻唑啉酮类防腐剂[J].化学分析计量,2018,27(2):9-13.
YAO B B,BAO L,HAN F,et al. Determination of 5 isothiazolinone preservatives in wet wipes by ultra-performance liquid chromatography-tandem mass spectrometry[J]. Chemical analysis and meterage,2018,27(2):9-13. 

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