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SupelcleanTMLC-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 ACQUITYTMBEH 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0.01～0.05μg·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。
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.
出处
《理化检验（化学分册）》
CAS
CSCD
北大核心
2013年第6期720-724,共5页
Physical Testing and Chemical Analysis(Part B:Chemical Analysis)
基金
浙江省质检系统科研计划项目(20080228)
