目的 建立高效液相色谱法测定塑料类食品接触材料及制品中双氯酚迁移量的方法,为有效管控塑料类食品接触材料及制品中双氯酚的风险提供技术支持。方法 对液相色谱条件、前处理方法进行优化,橄榄油浸泡液经乙腈提取,Xbridge C18色谱柱分离后,采用液相色谱法定量;水、4%乙酸、10%乙醇、20%乙醇、50%乙醇和95%乙醇（百分数均为体积分数）浸泡液直接进样,均以外标法定量。结果 水、4%乙酸、10%乙醇、20%乙醇、50%乙醇和95%乙醇浸泡液中双氯酚含量线性范围均为0.50~20.00 mg/L,相关系数（r2）均大于0.999 5,检出限均为0.20 mg/L,定量限均为0.50 mg/L;橄榄油浸泡液中双氯酚含量线性范围为1.00~20.00 mg/kg,相关系数（r2）为0.999 9,检出限为0.50 mg/kg,定量限为1.00 mg/kg。在水、4%乙酸、10%乙醇、20%乙醇、50%乙醇和95%乙醇浸泡液中添加质量浓度水平为0.5、1、20 mg/L,加标回收率均为92.06%~102.0%,相对标准偏差（RSD）小于10%。在橄榄油浸泡液中添加浓度水平为1、5、20 mg/kg,加标回收率均为97.27%~100.7%,相对标准偏差（RSD）小于10%。结论 该方法具有操作简单、线性范围好、灵敏度和准确度高等优点,适用于塑料类食品接触材料及制品中双氯酚迁移量的检测。
Abstract
The work aims to establish a high-performance liquid chromatography (HPLC) method for determining the migration of dichlorophen in plastic food contact materials and articles, to provide technical support for effectively controlling the risks of dichlorophen in plastic food contact materials and articles. The liquid chromatographic conditions and sample pretreatment procedures were optimized. Olive oil was used as a food simulant, and the soaking solution was extracted with acetonitrile. The separation was performed on an Xbridge C18 column, followed by quantification using HPLC. For soaking solutions of water, 4% acetic acid, 10% ethanol, 20% ethanol, 50% ethanol, and 95% ethanol (mass fraction), direct injection was employed, with all samples quantified using the external standard method. For soaking solutions of water, 4% acetic acid, 10% ethanol, 20% ethanol, 50% ethanol, and 95% ethanol, the linear range of dichlorophen concentration was 0.50-20.00 mg/L, with correlation coefficients (r²) all exceeding 0.999 5. The limits of detection (LODs) were 0.20 mg/L, and the limits of quantification (LOQs) were 0.50 mg/L. For olive oil soaking solutions, the linear range was 1.00-20.00 mg/kg, with a correlation coefficient (r²) of 0.999 9, an LOD of 0.50 mg/kg, and an LOQ of 1.00 mg/kg. For soaking solutions of water, 4% acetic acid, 10% ethanol, 20% ethanol, 50% ethanol and 95% ethanol, the mass concentration levels of addition were 0.5, 1 and 20 mg/L respectively, the recovery rates were all 92.06%-102.0%, and the relative standard deviations (RSDs) were less than 10%. For olive oil soaking solutions, the concentration levels of addition were 1, 5, and 20 mg/kg, the recovery rates were all 97.27%-100.7%, and the relative standard deviations (RSDs) were less than 10%. The proposed method is simple, exhibits a good linear range, and demonstrates high sensitivity and accuracy, making it suitable for the detection of dichlorophen migration in plastic food contact materials and articles.
关键词
双氯酚 /
塑料类食品接触材料及制品 /
高效液相色谱法（HPLC） /
特定迁移量
Key words
dichloropheno /
plastic food contact materials and articles /
high-performance liquid chromatography (HPLC) /
specific migration amounts
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基金
厦门海关科研项目（2024XK22）; 福建省食品微生物与酶工程重点实验室开发基金项目（CM23070-4）
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