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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。

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 puri-fied 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,dilu-tion ratio,extraction time were optimized. Under the optimized conditions,the targets had good linearities( r2≥0. 999 2)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 pur-pose of quantitative detection. The analyses of real samples verified the reliability of this method.

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