饮料中6种塑化剂的GC-MS和HPLC测定方法比较  

Comparison of GC-MS and HPLC in determination of 6 kinds of PAEs in beverage

作　　者：湛社霞[1,2] 卢佑演 刘钢[1] 臧李纳[1] 冯竞[1] 孙世宏[1] 

机构地区：[1]广州市天河区疾病预防控制中心,广东广州510655 [2]中国科学院广州地球化学研究所,广东广州510640

出　　处：《中国卫生检验杂志》2014年第4期496-498,511,共4页Chinese Journal of Health Laboratory Technology

基　　金：广州市医药卫生科技项目(2012A011182)

摘　　要：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PALEs；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—C18SPE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 A GC - MS method was developed to determine 6 kinds of phthalate esters （PAEs） in beverage, and compared with HPLC method. Methods The 6 PAEs were extracted by solid phase extraction and ultrasonic solvent extraction. The chromatographic conditions and sample pretreatment methods were optimized to determine 6 kinds of PAEs in beverage by GC -MS and HPLC respectively. The precision, accuracy, correlation coefficients and minimum detectable concentrations of two methods were compared. Results After ultrasonic solvent extraction, HPLC was available for determination of the 6 PAEs in samples; while based on ODS -C18 SPE, both GC -MS and HPLC were available for determination of 6 PAEs in samples. The correlation coefficients of the two methods were above 0. 999, the relative standard deviations were below 5% and the recov- eries were between 95% and 105%. HPLC had high precision, good hnearity, and lower lowest detection limit than GC - MS. Conclusion GC - MS method is suitable for analyzing the samples containing high levels of PAEs. HPLC is better for routine detection of PAEs in beverage, due to easy operation, accurate quantitation and less interference.

关 键 词：高效液相色谱法(HPLC) 气相色谱-质谱法(GC—MS) 饮料 邻苯二甲酸酯(PAEs) 

分 类 号：O657.7[理学—分析化学]