气相色谱法测定异山梨醇改性聚对苯二甲酸乙二醇酯制品中异山梨醇的迁移量

Determination of the migration of isosorbide in isosorbide modified polyethylene terephthalate products by gas chromatography

中文关键词:  异山梨醇  迁移量  改性聚对苯二甲酸乙二醇酯  食品接触材料  气相色谱法

英文关键词:isosorbide  migration  modified polyethylene terephthalate  food contact material  gas chromatography

中文摘要:

      目的 建立气相色谱-氢火焰离子化检测器法(gas chromatography-flame ionization detector, GC-FID)测定异山梨醇改性聚对苯二甲酸乙二醇酯(polyethylene terephthalate, PET)制品中异山梨醇迁移量的方法。方法 考察不同色谱条件对目标物异山梨醇分离度的影响, 选择HP-5作为分离柱, 260 ℃为进样口温度; 考察不同前处理方法对浸泡液中异山梨醇提取的效果, 橄榄油浸泡液经甲醇提取、正己烷净化并过滤后上机分析, 95%乙醇和异辛烷浸泡液经过滤后直接上机测定, 其他食品模拟物浸泡液用甲醇稀释后直接上机分析; 外标法定量。结果 异山梨醇在2.5~40.0 mg/L(水性模拟物)、0.6~10.0 mg/L(油脂替代溶剂模拟物)和1.5~25.0 mg/kg(油脂模拟物)浓度范围内具有良好的线性关系, 相关系数均大于0.995, 该方法对异山梨醇迁移量的检出限为0.8 mg/kg(水性模拟物)、0.2 mg/kg(油脂替代溶剂模拟物)和0.5 mg/kg(油脂模拟物), 定量限为2.5 mg/kg(水性模拟物)、0.6 mg/kg(油脂替代溶剂模拟物)和1.5 mg/kg(油脂模拟物), 加标回收率为92.0%~112.3%, 相对标准偏差为0.2%~4.3% (n=6)。结论 该方法线性关系良好, 精密度、灵敏度和准确度高, 能够满足改性PET制品中异山梨醇迁移量的检测需求。

英文摘要:

      Objective To establish a method for the determination of migration of isosorbide in isosorbide modified polyethylene terephthalate (PET) products by gas chromatography-flame ionization detector (GC-FID). Methods The effects of different chromatographic conditions on the separation of isosorbide were investigated. HP-5 was selected as the separation column and 260 ℃ was selected as the injection port temperature. The effects of different pretreatment methods on the extraction of isosorbide from food simulants were investigated. The olive oil food simulant was extracted with methanol, purified with n-hexane and filtered before analyzed. The 95% ethanol and isooctane simulants were directly analyzed by the machine after filtered. Other food simulants were diluted with methanol and then directly analyzed by the machine. The external standard method was used for quantification. Results Isosorbide had a good linear relationship in the range of 2.5–40.0 mg/L (aqueous food simulants), 0.6–10.0 mg/L (substitute simulants) and 1.5–25.0 mg/kg (fatty food simulants), and the correlation coefficient was above 0.995. The limit of detection of this method for the migration of isosorbide was 0.8 mg/kg (aqueous food simulants), 0.2 mg/kg (substitute simulants) and 0.5 mg/kg (fatty food simulants). The limit of quantification was 2.5 mg/kg (aqueous food simulants), 0.6 mg/kg (substitute simulants) and 1.5 mg/kg (fatty food simulants). The spiked recoveries were 92.0%–112.3%, and the relative standard deviation was 0.2%–4.3% (n=6). Conclusions This method has good linearity, high precision, sensitivity and accuracy, and can meet the detection requirements of isosorbide migration in modified PET products.