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目的研究测定饮料中6种邻苯二甲酸酯类(PAEs)塑化剂的GC-MS方法,并与HPLC测定方法进行比较。方法分别用固相萃取法(SPE)和超声溶剂浸提的提取样品中的6种PAEs;优化GC-MS测定PAEs的色谱和质谱条件;采用GC-MS和HPLC法测定饮料中的6种塑化剂,比较两种方法的精密度、准确度、相关系数和最低检出浓度。结果样品经超声溶剂浸提可用于HPLC测定6种PAEs,浸提液经ODS-C18 SPE小柱萃取后,用可用于GC-MS和HPLC测定;两种测定方法的相关系数r>0.999,相对准偏差可控制在5%以内,加标回收率在95%~105%。HPLC法精密度高,线性好,最低检出浓度低于GC-MS。结论 GC-MS法定性准确,适用于确证试验,可定量测定PAEs含量较高的样品;HPLC法定量准确,方法简便易行,干扰少,适用于饮料中低浓度PAEs的日常检测。
Objective To study the GC-MS method for the determination of six phthalates (PAEs) plasticizers in beverages and compare with the HPLC method. Methods Six kinds of PAEs were extracted by solid phase extraction (SPE) and ultrasonic solvent extraction respectively. The chromatographic and mass spectrometric conditions of PAEs were optimized by GC-MS. Six kinds of PAEs were determined by GC-MS and HPLC The comparison of the precision, accuracy, correlation coefficient and minimum detectable concentration of the two methods. Results The samples were extracted by ultrasonic solvent and used for the determination of six kinds of PAEs by HPLC. The extracts were extracted by ODS-C18 SPE cartridge and used for determination by GC-MS and HPLC. The correlation coefficients of the two methods were 0.999, Quasi-deviation can be controlled within 5%, spike recovery was 95% to 105%. High precision HPLC method, good linearity, the lowest detection concentration lower than GC-MS. Conclusion GC-MS method is qualitative and accurate, suitable for confirmatory test, which can quantitatively determine samples with high PAEs content. The HPLC method is accurate and accurate. The method is simple, easy to operate and has less interference. It is suitable for routine testing of low concentration PAEs in beverages.