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目的采用高效毛细管柱气相色谱法,分别使用顶空进样法和溶液直接进样法检测葡萄酒中甲醇的残留量,并进行方法比较。方法采用聚乙二醇为填料的毛细管色谱柱(30 m×0.53 mm,涂层厚1.0μm),程序升温的色谱条件:顶空进样法,平衡温度为60℃,平衡时间为30 min;溶液直接进样法:取样品进行蒸馏,制备供试品溶液,取溶液直接进样测定。结果顶空进样法,甲醇在79.15~633.2 mg/L范围内线性关系良好,检出限为1.58 mg/L,加标平均回收率为101.34%,RSD=1.21%(n=6)。对同种样品采用顶空进样和直接进样法进行测定,2种方法测定结果相同。结论 2种方法均可用于葡萄酒中甲醇的测定,但顶空进样法需要样品量少,无需样品前处理时繁琐的蒸馏过程,可缩短检测周期,提高工作效率。
OBJECTIVE To determine the residual amount of methanol in wine by headspace sampling and direct injection using capillary column gas chromatography, and to compare the methods. Methods The capillary column (30 m × 0.53 mm, thickness 1.0 μm) with polyethylene glycol as the filler was used. The chromatographic conditions of the program were as follows: the headspace sampling method, the equilibrium temperature of 60 ℃ and the equilibrium time of 30 min. Solution direct injection method: Take samples for distillation, prepare the test solution, take the solution directly into the sample. Results The headspace sampling method showed a good linear relationship between methanol and methanol in the range of 79.15-633.2 mg / L. The detection limit was 1.58 mg / L. The average recovery was 101.34% and RSD was 1.21% (n = 6). The headspace sampling and direct injection method were used to determine the same samples. The results of the two methods were the same. Conclusion Both of the two methods can be used for the determination of methanol in wine. However, the headspace method requires a small amount of sample, which eliminates the tedious distillation process during sample preparation, shortens the testing cycle and improves the work efficiency.