Guangdong Provincial Key Laboratory of import and export technical measures of animal, plant and food, Guangzhou 510623, China.
Guangzhou Customs District Technology Center, Guangzhou 510623, China.
Molecules. 2019 Oct 29;24(21):3894. doi: 10.3390/molecules24213894.
In this study, a target analytical approach using high-performance liquid chromatography-tandem mass spectrometry (HPLC-MS/MS) was developed to simultaneously determine six isothiazolinones containing 2-Methylisothiazol-3(2H)-one (MI), 5-Chloro-2-methyl-4-isothiazolin-3-one (CMI), 1,2-benzisothiazolin-3-one (BIT), 2-Octyl-3(2H)-isothiazolinone (OIT), Dichlorooctylisothiazolinone (DCOIT), and 2-methyl-1,2-benzisothiazolin-3-one (MBIT) in water-based adhesive used for food contact materials. The main factors affecting extraction efficiency such as extraction method, extraction time, extraction solvent, and solid-liquid ratio have been evaluated by using real adhesive samples. Multiple-reaction monitoring (MRM) was used for the qualitative and quantitative analyses of targeted isothiazolinones. This method was demonstrated as an effective and reliable technique for detecting multiple isothiazolinones with satisfactory recoveries (81.5~107.3%), and the limits of detection (LOD) and quantification (LOQ) were obtained at a low level. This method was validated and applied to the determination of six isothiazolinones in commercial water-based adhesives. The present results revealed that these adhesives contained a combination of isothiazolinones (BIT, MI, CMI, and MBIT) with the concentration ranging from 2.27 to 123.5 mg/kg. To our knowledge, it is the first time it has been reported that MBIT was detected in water-based adhesives used for food contact materials, which requires a further investigation for its migration to food and the risk to human health.
本研究建立了一种使用高效液相色谱-串联质谱法(HPLC-MS/MS)的目标分析方法,用于同时测定水基胶粘剂中 6 种含 2-甲基异噻唑啉-3-酮(MI)、5-氯-2-甲基-4-异噻唑啉-3-酮(CMI)、1,2-苯并异噻唑啉-3-酮(BIT)、2-辛基-3(2H)-异噻唑啉酮(OIT)、二氯辛基异噻唑啉酮(DCOIT)和 2-甲基-1,2-苯并异噻唑啉-3-酮(MBIT)的含量。采用实际胶粘剂样品,评估了提取方法、提取时间、提取溶剂和固液比等主要因素对提取效率的影响。采用多反应监测(MRM)法对目标异噻唑啉酮进行定性和定量分析。该方法被证明是一种有效的、可靠的技术,可用于检测多种异噻唑啉酮,回收率(81.5107.3%)令人满意,检测限(LOD)和定量限(LOQ)处于较低水平。该方法已得到验证,并应用于商业水基胶粘剂中 6 种异噻唑啉酮的测定。目前的结果表明,这些胶粘剂中含有异噻唑啉酮(BIT、MI、CMI 和 MBIT)的混合物,浓度范围为 2.27123.5mg/kg。据我们所知,这是首次报道 MBIT 存在于用于食品接触材料的水基胶粘剂中,需要进一步研究其向食品中的迁移及其对人类健康的风险。