大蒜油及其软胶囊中二烯丙基三硫醚等硫醚类化合物的分析

Analysis of diallyl trisulfide and other sulfide compounds in garlic oil and its soft capsules

目的：建立大蒜油及其软胶囊中二烯丙基三硫醚等硫醚类化合物的气相色谱-质谱联用（GC-MS）分析方法。方法：用水蒸气蒸馏法从新鲜大蒜中提取大蒜油,取大蒜油软胶囊内容物,用丙酮溶解并稀释,利用GC-MS法进行分析。GC条件：色谱柱DB-5MS（30 m×0.25 mm i.d.,0.25μm）;进样口温度190℃,升温程序：50℃保留1 min,以20℃/min升至160℃,保留5 min;氦气柱流量0.5 ml/min,总流量6.7 ml/min,柱头压48.4 kPa。MS条件：接口温度160℃;检测器电压1.0 kV;电离方式EI,电离能量70 eV;全扫描测定方式,扫描范围：m/z 30-350,扫描速度：500 amu/s;溶剂切除时间：3.0 min。结果：分析了从鲜蒜中提取的大蒜油和市售大蒜油软胶囊中二烯丙基三硫醚等甲基、烯丙基硫醚类有机化合物,用面积归一化法得到各化合物的相对含量。与大蒜油的分析结果进行比较,测定的8个样品中有1个未鉴定出任何硫醚类化合物。结论：利用本方法可以判断大蒜油软胶囊产品真伪与质量优劣。

Objective：To develop a gas chromatography-mass spectrometry（GC-MS） method for the analysis of diallyl trisulfide and sulfide compounds in garlic oil soft capsules.Methods：Garlic oil was extracted from fresh garlic by steam,the components of garlic oil soft capsule were dissolved and diluted by acetone and analysed by GC-MS fitted with DB-5MS fused silica capillary column（30 m×0.25 mm i.d.,0.25 μm）.Helium was used as carrier gas,the column and total flow rate were 0.5 and 6.7 ml/min respectively.The injection port and interface temperatures were 190 and 160℃,respectively.For gas chromatography,the oven temperature was set at 50℃ for 1 min then programmed at 20℃/min to 160℃ for 5 min.The solvent delay was 3.0 min.The detector voltage was 1.0 kV.Spectra were recorded in electron impact（EI）ionization mode（electron energy 70 eV） and the scan range was m/z 30-350 and the scan rate 500 amu/s.Results：Diallyl trisulfide and other sulfide compounds in garlic oil soft capsules on market had been qualitatively analysed by GC-MS and relative percentage concentration of these sulfide compounds were calculated by area normalization.The one of 8 soft capsule samples was identified to be non-sulfide compounds.Conclution：This method is simple,rapid and accurate.It can be used to determine the quality of garlic oil soft capsule by the identification of sulfide compounds and the concentration.