食品接触类纸、木制品中杀菌剂的测定

为测定食品接触类纸、木制品中杀菌剂的含量,建立高效液相色谱-串联质谱同时分析5种常用杀菌剂(5-氯-2-甲基-4-异噻唑啉-3-酮、2-甲基-4-异噻唑啉-3-酮、1,2-苯并异噻唑啉-3-酮、2-溴-2-硝基-1,3-丙二醇(溴硝醇)、五氯苯酚)的方法。样品经过甲醇超声提取后,以甲醇和水为流动相,根据保留时间不同,采用电喷雾正、负离子分段离子化,多反应监测模式,外标法进行分析。结果表明:5种杀菌剂在1~100μg/L范围内线性良好,方法的检测限在2.7~47μg/kg之间,加标回收率为82.88%~106.31%,相对标准偏差为0.5%~8.1%。该方法灵敏、准确,适合食品接触类纸、木制品中杀菌剂含量的分析,可为监测该类产品对食品安全的影响提供一种有效的测定方法。

Detection of Fungicides in Food Contact Paper and Wood Products

A method was developed to simultaneously analyze the contents of five bactericides including 2-methyl-4-isothiazoline-3-one (MI), 5-chloro-2-methyl-3(2H)-isothiazolone (CMI), 1,2-benzisothiazolin-3-one (BIT), pentachlorophenol (PCP) and bronopol, in food contact paper and wood products using high-performance liquid chromatography-tandem mass spectrometry (HPLC-MS/MS). Samples were extracted ultrasonically with methanol. The analytes were separated on an Eclipse Plus column C18 (4.6 mm × 100 mm, 3.5 μm) with methanol-water as the mobile phase. The multiple reaction monitoring (MRM) mode was applied to qualitatively analyze the five bactericides with a positive or negative electrospray ionization source according to their retention times and characteristic structures. The external standard method was used for quantitative analysis. The results showed that the linear ranges of the five bactericides were from 1 to 100 μg/L, and the limit of detection (LOD) of the method (RSN = 3) was in the range from 2.7 to 47 μg/kg. The mean recoveries for paper and wood samples at spiked concentration levels of 8 to 500 μg/kg ranged from 82.88% to 106.31%, and the precision relative standard deviations (n = 5) were 0.5%–8.1%. The method was applicable to analyze the contents of the five bactericides in food contact paper and wood products and therefore ensure food safety.