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建立了超高效液相色谱快速测定皮革中2-甲基异噻唑啉-3-酮(MI)、5-氯-2-甲基异噻唑啉-3-酮(CMI)和1,2-苯并异噻唑啉-3-酮(BI)3种防腐剂的方法。以甲醇为提取溶剂,40℃下超声提取25min,提取液经固相萃取柱净化后进行超高效液相色谱分析,外标法定量。方法的加标回收率在90%~98%之间,精密度RSD在0.7%~3%之间。MI、CMI、BI的检出限分别为0.05、0.10、0.02mg/kg,分析过程时间3min。对市售皮革制品进行了测试,部分样品中检出含有MI和CMI。
A rapid method for the determination of 2-methylisothiazolin-3-one (MI), 5-chloro-2-methylisothiazolin-3-one (CMI) And isothiazolin-3-one (BI) 3 preservatives. The extraction solvent was methanol and extracted by ultrasonic at 40 ℃ for 25 min. The extracts were purified by solid phase extraction (SPE) and analyzed by ultra performance liquid chromatography (HPLC). The spiked recoveries of the method ranged from 90% to 98%, and the precision RSD ranged from 0.7% to 3%. The detection limits of MI, CMI and BI were 0.05, 0.10 and 0.02 mg / kg, respectively, and the analysis time was 3 min. Leather products on the market were tested, some samples detected with MI and CMI.