静态顶空气相色谱法测定保健酒中的高级醇类和酯类

Determination of Purified Alcohols and Esters in Health Wine by Static Headspace-gas Chromatography

目的:建立静态顶空气相色谱-内标法测定保健酒中的高级醇类和酯类。方法:样品混匀,精密加入顶空瓶中,密塞,采用HP-INNOWAX毛细色谱柱(30 m×0.53 mm×1.00μm)分析,柱温采用程序升温,检测器为氢火焰离子化检测器(FID),检测器温度为250℃,进样口温度为200℃,载气为氮气。结果:高级醇类在20~600μg·ml^-1,酯类在4~100μg·ml^-1浓度范围内峰面积与质量浓度线性关系良好(r为0.9993~1.0000),平均回收率为70%~110%,RSD%小于10%(n=6),方法的检出限0.3~2.5μg·ml^-1,定量限为0.9~8.2μg·ml^-1。在优化条件下,对6批次样品进行检测,利用各待测物相对于乙酸正戊酯(内标)的相对校正因子,内标法计算其含量。6批次样品高级醇含量顺序为异戊醇>乙酸乙酯>异丁醇>已丙醇>仲丁醇,异戊醇含量最高。结论:该方法操作简单、耗时短、灵敏度高、稳定性好,应用于日常检测可大大降低检测成本,缩短检测周期,具有实际应用价值。

Objective:To develop a method for the determination of purified alcohols and esters in health wine by using static headspace-gas chromatography internal standard method.Methods:The samples in headspace vial were directly injected into gas chromatography with the internal standard and separated on an HP-INNOWAX capillary column with temperature programming.The flame ionization detector(FID)was used at 250℃.The inlet temperature was 180℃with nitrogen as the carrier gas.Results:Under the optimal experimental conditions,the calibration curves within the range of 20-600μg·ml^-1 for the purified alcohols and 4^-100μg·ml^-1 for the purified esters were in good linearity with a correlation coefficient above 0.9993.The recoveries of the purified alcohols and esters were 70%^-110%with the RSDs no more than 10%(n=6).The limit of detection(LOD)ranged from 0.3μg·ml^-1 to 2.5μg·ml^-1,and the limit of quantification(LOQ)was 0.9-8.2μg·ml^-1.The above developed method was then utilized to analyze 6 batches of health wine in market.The components were quantified using the internal standard method.The order of purified alcohols content in six batches of samples was isopentylalcohol>ethy acetate>2-methl^-1-propanol>propanol 2-butanol.Isopentyl alcohol was with the highest content in the total amount of purified alcohols and esters.Conclusion:The results indicate that the method is simple,time-saving and environment friendly with high sensitivity and good reproducibility,and has practical application value due to its low-cost and short-circle for the routine analysis of purified alcohols and esters in health wine.