超高效液相色谱-串联质谱测定家用液体洗涤产品中异噻唑啉酮类防腐剂

建立了一种超高效液相色谱-串联质谱快速测定家用液体洗涤产品中4种异噻唑啉酮类防腐剂含量的分析方法。样品经甲醇超声提取、离心、过滤后用超高效液相色谱-串联质谱进行分析。色谱流动相为甲醇-水,梯度洗脱,在多反应监测(MRM)模式下测定,外标法定量。对前处理条件进行了优化,在优化条件下,4种异噻唑啉酮在10.0~500.0μg/L浓度范围内均呈良好的线性关系(r≥0.999),方法定量限均为0.05 mg/kg,平均回收率为81.2%~103.2%,相对标准偏差为2.23%~4.52%。该方法前处理简便快捷,灵敏度高,能快速准确测定家用液体洗涤产品中异噻唑啉酮种类及含量。

Determination of Isothiazolinones Preservatives in House-hold Detergents by Ultra-performance Liquid Chromatography-tandem Mass Spectrometry

A method based on ultra-performance liquid chromatography-tandem mass spectrometry (UPLC-MS/MS) for the simultaneous determination of isothiazolinone preservatives in house-hold detergents has been developed. After ultrasonic ex-traction with methanol, the isothiazolones in house-hold detergents were separated using methanol-water as mobile phases under gradient elution and analyzed by MS/MS in multiple reaction monitoring mode (MRM). The pretreatment were opti-mized. Under optimized conditions, the linear ranges of the 4 analytes were 10.0～500.0 μg/L with the correlation coeffi-cients (r) higher than 0.999, and the limits of quantification were 0.05 mg/kg. The recoveries of the 4 isothiazolinones in house-hold detergents were in the range of 81.2%～103.2%,with the relative standard deviations (RSD) of 2.23%～4.52%. This method is rapid, sensitive and suitable for the quick determination of isothiazolinones preservatives in house-hold deter-gents.