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以甲醇为提取溶剂,在40℃下超声提取皮革及其制品中的异噻唑啉酮类防腐剂,提取液经固相萃取柱净化后,进行超高效液相色谱/静电场轨道阱高分辨质谱(UPLC/Orbitrap HRMS)分析,从而建立了1个快速测定皮革及其制品中5种异噻唑啉酮类防腐剂含量的UPLC/Orbitrap HRMS方法。5种异噻唑啉酮类防腐剂的色谱分离在Hypersil GOLD色谱柱(100 mm×2.1 mm×1.9μm)上完成,流动相为甲醇/0.1%甲酸水溶液,梯度洗脱。采用电喷雾正离子(ESI+)模式电离,在m/z 100~m/z 500范围内进行一级质谱扫描。利用保留时间和准分子离子峰的精确质量数进行定性,5种异噻唑啉酮类防腐剂的质量准确度误差均小于2×10-6;利用提取离子色谱图的峰面积进行定量,外标法定量。在一定质量浓度范围内,提取离子色谱图的峰面积均与其质量浓度线性相关,线性相关系数均大于0.999。在信噪比为3(S/N=3)的条件下,5种异噻唑啉酮类防腐剂的检出限均为0.1μg/kg。在3个添加浓度水平下,平均添加回收率为81.5%~93.5%,其相对标准偏差为3.9%~9.9%。采用该方法对市售皮革及其制品进行测定,结果在部分样品中检出2-甲基-4-异噻唑啉-3-酮(MI)和5-氯-2-甲基-4-异噻唑啉-3-酮(CMI)。
Using methanol as extraction solvent, the isothiazolinone preservatives in leather and its products were sonicated at 40 ℃. The extracts were purified by solid-phase extraction (SPE) column and analyzed by ultra performance liquid chromatography / electrostatic field orbital trap high resolution mass spectrometry (UPLC / Orbitrap HRMS) analysis, a UPLC / Orbitrap HRMS method for the rapid determination of five isothiazolinone preservatives in leather and its products was established. The chromatographic separation of five isothiazolinone preservatives was performed on a Hypersil GOLD column (100 mm × 2.1 mm × 1.9 μm) using a mobile phase of methanol / 0.1% formic acid in water with gradient elution. The first order MS scan was performed in the range of m / z 100 ~ m / z 500 by electrospray positive ion (ESI +) mode. The retention time and the exact mass number of quasi- ion ion peak were used for characterization. The mass accuracy errors of the five isothiazolinone preservatives were both less than 2 × 10-6. The peak area of extracted ion chromatogram was used for quantification. Legal quantity. In a certain range of mass concentration, the peak areas of extracted ion chromatograms were linearly correlated with their mass concentrations, and the linear correlation coefficients were all greater than 0.999. Under the condition of signal to noise ratio of 3 (S / N = 3), the detection limits of the five isothiazolinone preservatives are both 0.1μg / kg. The average recoveries were 81.5% -93.5% with relative standard deviations (3.9% -9.9%) at the three concentrations. The method was applied to the determination of commercially available leather and its products. As a result, 2-methyl-4-isothiazolin-3-one (MI) and 5-chloro-2-methyl-4- Thiazoline-3-one (CMI).