气相色谱法测定保健食品中二烯丙基二硫醚和二烯丙基三硫醚

Determination of diallyl disulfide and diallyl trisulfide in health food by gas chromatography

建立检测保健食品中二烯丙基二硫醚和二烯丙基三硫醚含量的气相色谱分析方法。将样品用正己烷溶解,稀释定容后,用0.22μm滤膜过滤,采用气相色谱法进行测定。以岛津SH-1色谱柱(30 m×0.32 mm,0.25μm)作为分析柱,样口温度、检测器温度均为210℃,以氮气为载气,流量为1 mL/min,分流比为10∶1,进样体积为1μL;升温程序:初始温度为100℃,保持5 min,以20℃/min升至180℃,保持13 min,利用外标法得到各化合物相对含量。经升温程序优化后,二烯丙基二硫醚和二烯丙基三硫醚保留时间分别提前至3 min和7 min且分离度达到要求。采用方法学考察进行分析,结果表明二烯丙基二硫醚和二烯丙基三硫醚的质量浓度在0.5~2.5 mg/mL范围内与色谱峰面积线性关系良好,相关系数分别为0.998和0.9999,加标回收率为95.5%~105.3%,二烯丙基二硫醚和二烯丙基三硫醚测定值的相对标准偏差分别为1.1%、1.3%(n=6)。该方法操作简单,适用于保健食品中二烯丙基二硫醚和二烯丙基三硫醚含量的测定。

A gas chromatographic method was established for the determination of diallyl disulfide and diallyl trisulfide in healthy food.The sample was dissolved in n-hexane,diluted and sized,and filtered with 0.22μm filter membrane and determined by gas chromatography.Shimadzu SH-1 column(30 m×0.32 mm,0.25μm)was used as the analytical column,the sample port temperature and the detector temperature were all 210℃,nitrogen was used as the carrier gas with the flow rate of 1 mL/min,the shunt ratio was 10∶1,the volume of injection was 1μL,and the heating procedure was as follows:the initial temperature was 100℃,remaining for 5 min,then increased to 180℃at 20℃/min,remaining for 13 min,and the relative content of each compound was obtained by external standard method.The retention time of diallyl disulfide and diallyl trisulfide was advanced to 3 min and 7 min respectively after optimization of the heating procedure,and the separation degree met the requirements.The results showed that the mass concentration of diallyl disulfide and diallyl trisulfide had good linear relationship with the chromatographic peak area in the range of 0.5-2.5 mg/mL.The correlation coefficients of diallyl disulfide and diallyl trisulfide were 0.998 and 0.9999,respectively.The recoveries were 95.5%-105.3%,the relative standard deviations of the contents of diallyl disulfide and diallyl trisulfide were 1.1%and 1.3%(n=6),respectively.This method is simple,and it is suitable for the determination of diallyl disulfide and diallyl trisulfide in dietary supplement.