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高效液相色谱法测定水性胶粘剂中三种异噻唑啉酮类杀生剂

[Determination of three isothiazolinone biocides in water-borne adhesives by high performance liquid chromatography].

作者信息

Zhou Xiao, Li Xiaolan, Chen Zhiyan, Ye Changwen, Zhou Yun, Meng Dongling

出版信息

Se Pu. 2015 Jan;33(1):75-9. doi: 10.3724/sp.j.1123.2014.10012.

Abstract

A rapid high performance liquid chromatography (HPLC) method was developed for the quantitative analysis of three isothiazolinone biocides (2-methyl-4-isothiazolin-3-one (MI), 5-chloro-2-methyl-4-isothiazolin-3-one (CMI) and 1, 2-benzylisothiazolin-3-one (BIT)) in water-borne adhesives. The sample was extracted with methanol-water (1:1, v/v), and purified by centrifugation and filtration. The isothiazolones were separated on a C18 column with methanol-water as mobile phases under gradient elution and detected with a diode array detector (DAD). The pretreatment factors such as extraction solvent, extraction method, dilution ratio, extraction time were optimized. Under the optimized conditions, the targets had good linearities (r2H > or = 0.9992) in the range of 0.25-10.0 mg/L. The recoveries were between 92% and 103% with the relative standard deviations not more than 4%. The limits of detection (LODs) were between 0.43 mg/kg and 1.14 mg/kg. The limits of quantification (LOQs) were between 1.44 mg/kg and 3.81 mg/kg. The results showed that the method can achieve the purpose of quantitative detection. The analyses of real samples verified the reliability of this method.

摘要

建立了一种快速高效液相色谱(HPLC)法,用于定量分析水性胶粘剂中的三种异噻唑啉酮类杀生剂(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))。样品用甲醇-水(1:1,v/v)萃取,经离心和过滤纯化。异噻唑啉酮类化合物在C18柱上以甲醇-水为流动相进行梯度洗脱分离,并用二极管阵列检测器(DAD)检测。对萃取溶剂、萃取方法、稀释比、萃取时间等预处理因素进行了优化。在优化条件下,目标物在0.25 - 10.0 mg/L范围内具有良好的线性关系(r2H≥0.9992)。回收率在92%至103%之间,相对标准偏差不超过4%。检测限(LOD)在0.43 mg/kg至1.14 mg/kg之间。定量限(LOQ)在1.44 mg/kg至3.81 mg/kg之间。结果表明,该方法能够达到定量检测的目的。实际样品分析验证了该方法的可靠性。

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