三种方法测定液体型保健食品中苯甲醇的含量

Three methods in determination of benzyl alcohol in liquid health food

目的:建立气相色谱法(GC)、高效液相色谱法(HPLC)、气相色谱-质谱联用法(GC-MS)三种测定液体型保健食品中苯甲醇含量的方法。方法:GC采用DB-WAX毛细管色谱柱,程序升温,氢火焰离子检测器(FID)测定;HPLC采用C18色谱柱,甲醇和20mmol/L乙酸铵溶液为流动相梯度洗脱,二极管阵列检测器(波长210nm)测定;GC-MS采用DB-624UI毛细管质谱柱,离子化方式EI,程序升温,全扫模式(m/z30~300)与SIM模式(79.0,107.0,108.0)定性与定量测定。比较了三种方法的线性、精密度、准确度和检出限。结果:GC在50~500μg/mL范围内线性关系良好,回收率在95%~100%之间,检出限为5mg/kg;HPLC在10~1000μg/mL范围内线性关系良好,回收率在95%~100%之间,检出限为10mg/kg;GC-MS在0.4~20μg/mL范围内线性关系良好,回收率在90%~100%之间,检出限为2mg/kg。结论:GC、HPLC、GC-MS三种方法对样品中苯甲醇含量的测定结果一致,且操作简单,稳定性好,GC-MS可作为苯甲醇的定性判定方法。

Objective:Three methods for determination of benzyl alcohol in liquid health food were established,including gas chromatography(GC),high performance liquid chromatography(HPLC)and gas chromatographymass spectrometry(GC-MS).Methods:GC was determined by DB-WAX capillary column with FID.HPLC was performed with C18 column,methanol and 20 mmol/L ammonium acetate solution as mobile phase gradient elution,and measured by diode array detector(210 nm).GC-MS was determined qualitatively and quantitatively by DB-624 UI capillary mass spectrometry column,ionization method EI,temperature-programmed,full sweep mode(m/z 30~300)and SIM mode(79.0,107.0,108.0).The linearity,precision,accuracy and detection limit of the three methods were compared.Results:GC had a good linear relationship in the range of 50~500μg/mL,the recovery was between 95%~100%,and the detection limit was 5 mg/kg.HPLC had a good linear relationship in the range of 10~1000μg/mL,the recovery was between 95%~100%,and the detection limit was 10 mg/kg.GC-MS had a good linear relationship in the range of 0.4~20μg/mL,the recovery was between 90%~100%,and the detection limit was 2 mg/kg.Conclusion:GC,HPLC and GC-MS have the consistent results of benzyl alcohol content.Three methods are simple operation with good stability.GC-MS could also be used as a qualitative determination method for benzyl alcohol.