色谱 ›› 2015, Vol. 33 ›› Issue (1): 75-79.DOI: 10.3724/SP.J.1123.2014.10012

• 技术与应用 • 上一篇    下一篇

高效液相色谱法测定水基胶黏剂中3种异噻唑啉酮类杀菌剂

周晓1, 李小兰1, 陈志燕1, 叶长文2, 周芸1, 孟冬玲1   

  1. 1. 广西中烟工业有限责任公司, 广西 南宁 530001;
    2. 中国烟草总公司郑州烟草研究院, 河南 郑州 450001
  • 收稿日期:2014-10-20 修回日期:2014-11-07 出版日期:2015-01-08 发布日期:2014-12-26
  • 通讯作者: 周晓

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

ZHOU Xiao1, LI Xiaolan1, CHEN Zhiyan1, YE Changwen2, ZHOU Yun1, MENG Dongling1   

  1. 1. China Tobacco Guangxi Industrial Limited Liability Company, Nanning 530001, China;
    2. Zhengzhou Tobacco Research Institute of China National Tobacco Corporation, Zhengzhou 450001, China
  • Received:2014-10-20 Revised:2014-11-07 Online:2015-01-08 Published:2014-12-26

摘要:

建立了一种高效液相色谱法快速测定水基胶黏剂中3种异噻唑啉酮类杀菌剂(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-苯并异噻啉-3-酮(BIT))的分析方法.样品经甲醇-水(1: 1, v/v)溶液振荡提取、离心、过滤后,采用高效液相色谱-二极管阵列检测器检测,C18色谱柱分离,流动相为甲醇-水,梯度洗脱.对前处理条件(包括萃取溶剂、提取方式、稀释倍数、提取时间)进行了优化.在优化实验条件下,样品中的异噻唑啉酮在0.25~10.0 mg/L范围内呈良好的线性关系(r2≥0.9992),加标回收率在92%~103%之间,相对标准偏差不高于4%,检出限为0.43~1.14 mg/kg,定量限为1.44~3.81 mg/kg.结果表明该方法能达到定量检测的目的.将该方法应用于实际样品的检测,结果可靠.

关键词: 高效液相色谱, 水基胶黏剂, 异噻唑啉酮类杀菌剂

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 (r2≥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.

Key words: high performance liquid chromatography (HPLC), isothiazolone biocides, water-borne adhesives

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