摘要
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(30m×0.53mm,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30min;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—633.2mg/L范围内线性关系良好,检出限为1.58mg/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 establish methods for the analysis of methanol in wine by gas chromatography ( GC } by using head-space injection and direct injection of solution, and compare the results. [ Methods ] A capillary column ( 30 m × 0.53 ram, film coat 1.0 μm ) packed with polyethylene glycol was used with the programmed column temperature. For head space-GC method, the sam- ples had been equilibrated at 60 ℃ for 30 minutes. For direct injection of solution-GC method, and the samples were distilled to prepare the test solution and the solution were injected for the analysis. [ Results] For head-space injection, the calibration curve of methanol showed good linearity in the range of 79. 15-633.2 mg/L, the detection limit was 1. 58 mg / L, recoveries were 101.34%, and RSD = 1.21% ( n = 6 ). For the determination of the same sample, both 2 methods had the same results. [Condusion] The 2 injection methods can be used to detect the methanol in wine, while the head-space injection method needs less sam- ple, without complex distillation during the preparation of test solution, thus, it shortens testing cycle and improves work efficiency.
出处
《职业与健康》
CAS
2014年第9期1180-1182,共3页
Occupation and Health
关键词
GC顶空进样法
溶液直接进样法
葡萄酒
甲醇
Head space-GC method
Direct injection of solution-GC method
Wine
Methonol