超高效液相色谱-串联质谱法测定火麻食品中特征大麻酚
UHPLC-MS/MS Determination of Characteristic Cannabinol in Hemp Food
-
摘要: 提出了超高效液相色谱-串联质谱法测定火麻食品中特征大麻酚含量的方法。样品经甲醇提取,过SupelcleanTM LC-Alumina-N固相萃取柱净化后,将洗脱液氮吹至近干,残渣用甲醇-水(77+23)溶液溶解。采用Waters ACQUITYTM BEH C18色谱柱分离,以甲醇和水为流动相梯度洗脱。质谱测定中采用负离子电离方式,多反应监测模式。方法检出限(3S/N)在0.01~0.05 μg·kg-1之间。用标准加入法做回收试验,测得平均回收率在76.1%~105%之间,测定值的相对标准偏差(n=6)在6.5%~15%之间。Abstract: UHPLC-MS/MS was applied to the determination of residual amounts of characteristic cannabinol in hemp food. Sample was extracted with methanol, which was concentrated and purified by SupelcleanTM LC-Alumina-N solid-phase extraction column. The column was eluted with petroleum ether and the eluate was evaporated to near dryness by N2-blowing and the residue was dissolved with methanol-water (77+23) mixture. Waters ACQUITYTM BEH C18 chromatographic column was used for separation, using mixtures of methanol and water as mobile phase in the gradient elution. ESI with negative ionization mode and multi-reactions monitoring mode were used in the MS/MS analysis. Values of detection limits (3S/N) found were in the range of 0.01-0.05 μg·kg-1. Test for recovery was made by standard addition method, giving values of recovery and RSD′s (n=6) in the ranges of 76.1%-105% and 6.5%-15% respectively.