HPLC测定水性建筑涂料乳液中异噻唑啉酮类杀菌剂

Determination of Isothiazolinones Biocides in Polymer Emulsion for Waterborne Architectural Coatings by High Performance Liquid Chromatography(HPLC)

建立了一种高效液相色谱法(HPLC)快速测定水性建筑涂料乳液中3种异噻唑啉酮类杀菌剂[2-甲基-4-异噻唑啉-3-酮(MIT)、5-氯-2-甲基-4-异噻唑啉-3-酮(CMIT)和1,2-苯并异噻唑啉-3-酮(BIT)]的分析方法。样品经甲醇-水(1∶1,V/V)溶液超声提取、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-乙酸铵溶液,梯度洗脱。对前处理条件(包括提取溶剂、提取方式、提取时间)进行了优化。在优化的实验条件下,样品溶液中的MIT、CMIT在0.05~20μg/m L浓度范围内、BIT在0.10~40μg/m L浓度范围内呈良好的线性关系(r 2≥0.999 8),基质加标回收率在90.10%~102.53%,相对标准偏差不高于3%,方法的检出限为0.10~0.15 mg/kg,定量限为0.33~0.50 mg/kg。该方法灵敏度高,重复性好,回收率满意,可应用于建筑涂料乳液实际样品的快速测定,结果可靠。

In this dissertation, we established the ttPLC method for determination of three isothiazolmones biocide contents in polymer emulsion lbr waterborne architectural coatings, namely 5-chloro-2-methyl-4-isothiazolin-3-one （CMIT）, 2-methyl- 4-isothiazolin-3-one （MIT） and 1,2-benzisothiazolin-3-one（BIT）. After being ultrasonically extracted, centrifuged and filtered with methanol-water （1 ： 1, V/V）, the samples were tested by high-effective liquid chromatogram -- diode array detector. After separation of CI8 chromatographic column, the mobile phase was methanol - ammonium acetate solution, which went through gradient elution. The pre-treatment conditions, such as extraction solvent, method and time, were optimized. Under the optimized conditions, the MIT and CMIT had good linearity （r2≥0.999 also had good linearity （r2=0.999 8） in the concentration range 90.10% and 102.53%. The relative standard deviations were not 8） in the concentration range of 0.05- 20 Mg/mL and the BIT of 0.10 - 40 Mg/mL The recovery of the subsrate was between more than 3 %. The limits of detection were between 0.10 mg/kg and 0.15 mg/kg. The limits of quantification were between 0.33 mg/kg and 0.50 mg/kg. The results showed that the method had the advantages of high sensitivity, good repeatability and high recovery and could be used lbr quickly testing actual samples of architectural coatings emulsion with high reliability