ASE-GC-NCI-MS测定食品接触塑料及纸制品中的短链氯化石蜡

Determination of Short Chain Chlorinated Paraffins in Food Contact Plastic and Paper Products by ASE-GC-NCI-MS

目的建立用于食品接触塑料及纸制品中短链氯化石蜡(SCCPs)含量测定的快速溶剂萃取-气相色谱-负化学电离源质谱法(ASE-GC-NCI-MS)。方法采用加速溶剂萃取法对食品接触塑料及纸制品中的SCCPs进行处理,萃取溶剂为正己烷-二氯甲烷,萃取温度为80℃,静态萃取时间10 min;采用浓硫酸净化法对萃取溶液进行净化处理;采用气相色谱-质谱法在负化学电离模式、全扫描模式、离子源温度为180℃等条件下对样品中的SCCPs进行定性与定量测定。结果氯的质量分数在58.7%~64.3%范围内时,SCCPs的总体响应因子与实测氯含量呈良好的线性关系,线性相关系数R^2为0.9765,检出限为20mg/kg,加标回收率为86.3%~95.3%,相对标准偏差(RSD)为3.3%~5.2%(日内),4.8%~8.1%(日间)。结论该方法操作简便、准确度好、灵敏度高、检出限低,可用于食品接触塑料及纸制品中SCCPs的实际检测。

The work aims to establish the accelerated solvent extraction-gas chromatography-negative chemical ionization-mass spectrometry(ASE-GC-NCI-MS)used to determine short chain chlorinated paraffins(SCCPs)in food contact plastic and paper products.Accelerated solvent extraction was used to extract SCCPs from food contact plastic and paper products.The extraction solvent was n-hexane-dichloromethane,the extraction temperature was 80℃,and the static extraction time was 10 min.Then,concentrated sulfuric acid was adopted to purify the extracted solution.SCCPs in the sample were qualitatively and quantitatively detected by gas chromatography-mass spectrometry under negative chemical ionization mode,full scan mode,and at 180℃(ionization source temperature).In the range of 58.7%~64.3%(mass fraction)chlorine,the total response factor of SCCPs and measured chlorine content had a good linear relationship,with a linear correlation coefficient(R2)of 0.9765.The limit of detection was 20 mg/kg.The recoveries ranged from 86.3%to 95.3%,with relative standard deviations(RSD)of 3.3%~5.2%(intra-day)and 4.8%~8.1%(inter-day).Featured by convenient operation,good accuracy,high sensitivity and low detection limit,the proposed method can be used for the detection of SCCPs in food contact plastic and paper products.