白泽清.UPLC–MS/MS法测定聚亚苯基砜奶瓶4,4′–联苯二酚迁移量[J].包装工程,2022,43(19):167-172.
BAI Ze-qing.Determination of 4,4′-Dihydroxybiphenyl Migrated from Polyphenylene Sulfone Feeding-bottles by UPLC-MS/MS[J].Packaging Engineering,2022,43(19):167-172. |
| UPLC–MS/MS法测定聚亚苯基砜奶瓶4,4′–联苯二酚迁移量 |
| Determination of 4,4′-Dihydroxybiphenyl Migrated from Polyphenylene Sulfone Feeding-bottles by UPLC-MS/MS |
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| DOI：10.19554/j.cnki.1001-3563.2022.19.019 |
| 中文关键词: 聚亚苯基砜奶瓶 4,4′–联苯二酚 迁移量 超高效液相色谱–串联质谱 |
| 英文关键词: polyphenylene sulfone feeding-bottles 4,4′-dihydroxybiphenyl migration quantity UPLC-MS/MS |
| 基金项目:国家市场监督管理总局科技计划(2019MK081) |
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| 中文摘要: |
| 目的 提出聚亚苯基砜(PPSU)奶瓶4,4′–联苯二酚迁移量的超高效液相色谱–串联质谱分析方法(UPLC–MS/MS)，为婴幼儿食品包装质量安全测试方法提供依据。方法 在70 ℃、2 h条件下，采用体积分数50%的乙醇溶液(食品模拟物)对样品进行迁移实验，采用C18色谱柱分离，以超纯水和甲醇为流动相梯度洗脱，通过电喷雾电离源(ESI)负离子模式和多反应监测(MRM)进行采集、扫描，并进行定性和定量检测，采用外标法进行定量分析。结果 在优化条件下，目标物在5~200 µg/L内线性关系良好，相关系数(R2)大于0.999 9，检出限和定量下限分别为1.5 µg/L和5 µg/L。该方法的基质效应值为95.8%~114%，加标回收率为95.2%~105%，相对标准偏差(RSD)为1.0%~1.7% (n=6)。结论 该方法具有快速、准确且灵敏度高等特点，适用于PPSU奶瓶4,4′–联苯二酚迁移量的测定。 |
| 英文摘要: |
| The work aims to develop an ultra-performance liquid chromatograph-tandem mass spectrometry (UPLC-MS/MS) method for determination of 4,4′-dihydroxybiphenyl migrated from polyphenylene sulfone feeding-bottles (PPSU) to provide test method basis of quality and safety of infant food packaging. The 50% (V/V) ethanol/water solution was chosen as food simulant to conduct the migration tests under testing conditions of (70 ℃, 2 h), and the analytes were separated on a C18 chromatographic column by gradient elution with a mobile phase consisting of deionized water and methyl alcohol. The qualitative and quantitative testing of 4,4′-dihydroxybiphenyl were carried out by multiple-reaction monitoring (MRM) collecting and scanning with electrospray ionization (ESI) source operating in the negative ionization mode, and external standard method was used for quantitative detection. Under the optimized conditions, there was a good linear relationship (with correlation coefficient R2>0.999 9) for the analyte in the concentration range of 5-200 µg/L. The limit of detection (LOD) and the limit of quantitation (LOQ) were 1.5 µg/L and 5 µg/L, respectively. The matrix effects of the method were in the range of 95.8%-114%, and the recovery range was 95.2% to 105%, and the relative standard deviation (RSD) was 1.0%-1.7% (n=6). This method is suitable for rapid determination of migration quantity of 4,4′-dihydroxybiphenyl in PPSU feeding-bottles, with the advantages of good accuracy and high sensitivity. |
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