不同种类固相萃取柱对特医食品中香料含量结果的影响

在比较不同种类固相萃取柱净化效果上优化前处理条件,建立一种测定特医食品(FSMP)中11种人工合成香料的检测方法。对比Agilent Poroshell 120 SB-AQ和Ultimate LP-C₁₈2种色谱柱对11种人工合成香料的分离情况,研究Welchrom P-SAX、Welchrom C₁₈E、Captive EMR-Lipid、Welchrom P-WAX及Poly-Sery HLB这5种固相萃取小柱的回收率及不同配方食品基质的前处理提取方法。结果表明,选择不同类型SPE柱直接影响方法的灵敏度和精密度,Welchrom C₁₈E柱和Captive EMR-Lipid小柱均具有良好回收率,但Captive EMR-Lipid小柱方法的检出限比Welchrom C₁₈E柱的低1倍,且Welchrom C₁₈E柱的除脂效果不及Captive EMR-Lipid柱,滤出液较为浑浊,影响上机测定。5种固相萃取柱中,采用Captive EMR-Lipid固相萃取柱,11种标准混合物在高、中、低的添加水平的回收率为84%~107%(n=3)。试验从基层实验室实际应用需要考虑,针对不同基质特医食品样品,建立一种同时测定11种人工香料的提取和分析方法,该方法操作简单便捷,准确度高,易于批量处理,可用于特医食品中人工合成香料的筛查检测。

Effect of Different Kinds of SPE Columns on the Results of Flavor Content in Special Medical Foods

A method for the determination of 11 synthetic flavors in FSMP was established by comparing the purification effects of different solid phase extraction columns.The separation of 11 synthetic fragrances by agilent poroshell 120 SBAQ and ultimate LP-C₁₈was compared,and the recovery of five solid-phase extraction columns(Welchrom p-sax,Welchrom C₁₈E,captive EMR-Lipid,Welchrom p-wax and poly serve HLB)and the pre-treatment extraction methods of different formula food matrix were studied.Results showed that different types of SPE columns directly affected the sensitivity and precision of the method.Welchrom C₁₈E column and captive EMR-Lipid columns had good recoveries,however,the detection limit of captive EMR-Lipid column method was 1 time lower than that of Welchrom C₁₈E column,the degreasing effect of Welchrom C₁₈E column was not as good as that of captive EMR-Lipid column,and the filtrate was turbid,which affected the on-line measurement.Among the five solid-phase extraction columns,the recovery of 11 standard mixtures at high,medium and low levels reached 84%to 107%(n=3).Considering the needs of practical application in the basic laboratory,a method for the simultaneous determination of 11 artificial flavors was established for the samples of special medical foods with different matrices.It was simple and convenient to operate,high accuracy,and easy to batch process.It could be used for the screening and detection of artificial flavors in FSMP.