HPLC法检测保健食品中大蒜素的含量

Determination of allicin in dietary supplement by HPLC

选取固体类、液体类、半固体类3类保健食品为研究对象,考察了提取溶剂、乙醇体积分数、提取温度、色谱柱对检测结果的影响,建立了高效液相色谱法测定保健食品中大蒜素主要功效成分二烯丙基三硫醚(diallyl trisulfide,DATS)、二烯丙基二硫醚(diallyl disulfide,DADS)的检测方法。试样以无水乙醇超声提取,经C18柱(250 mm×4.6 mm,5μm)分离;流动相为V(乙腈)∶V(水)=68∶32;流速1.0 mL.min-1;紫外检测波长240 nm;检出限DATS 2.0 mg.kg-1,DADS 1.5 mg.kg-1。大蒜素浓度在6.26～6 262.24 mg.kg-1范围内呈良好线性关系(r=0.9999),分别对固体类、液体类、半固体类样品进行高低两水平添标回收试验,平均回收率DATS为97.6%～105.8%,DADS的回收率为95.3%～105.4%。重复性变异系数1.5%～2.7%,再现性变异系数3.8%～5.6%。同时将HPLC与GC分析相比较,结果无显著性差异。该方法简便快速,准确可靠,适用于多种保健食品中大蒜素含量的检测。

Solid, liquid and semi-solid dietary supplement were chosen as study subjects. High performance liquid chromatography （HPLC） method was developed to determine main active components, diallyl trisulfide （DATS） and diallyl disulfide （ DADS）, in dietary supplement. Effects of extract solvents, volume fraction of ethanol, temperature and chromatographic column on detection were studied. Samples were extracted with ethanol by ultrasonic, isolated by Cls column （250 mm×4. 6 mm, 5 μm） ; V （acetonitrile）： V （ H2 O） = 68：32 as mobile phase; The flow rate was 1.0 mL min-1 and the UV wavelength was 240 nm. The results indicated that the standard curves of allicin showed good linearity in the range ration of 6. 26 - 6262. 24 mg- L- 1 （ r = 0. 9999 ）, and the detection limits were 2. 0 mg. kg - 1 for DATS, 1.5 mg- kg - 1 for DADS. The mean recoveries of two samples standard addition test for three matrices at high and low levels were 97. 6% - 105.8% for DADS and 95. 3% - 105.4% for DATS. The relative standard de- viations of test repeatability were 1.5% - 2. 7%, and the relative standard deviations of test reproducibility were 3.8% -5.6%. Comparing the resuhs by HPLC and gas chromatography, there was no significant difference. This method is rapid and accurate for the determination of allicin in dietary supplement.