高效液相色谱柱后衍生法测定蜂王浆中的链霉素

Determination of streptomycin residue in royal jelly by high performance liquid chromatography with post-column derivatization

采用高效液相色谱柱后衍生法测定蜂王浆中的链霉素。样品用庚烷磺酸钠的酸性溶液进行提取,通过LC-18柱和WCX柱两次固相萃取达到净化的目的。该方法采用反相C8柱,以0.01mol/L的庚烷磺酸钠溶液和乙腈为流动相,在碱性条件下以1,2-萘醌-4-磺酸钠溶液为柱后衍生化试剂,用荧光检测器检测。该方法的线性范围为0.02～0.5mg/L,相关系数为0.9958,方法的检出限和定量限分别为为0.005mg/kg和0.01mg/kg,回收率范围为84.0%～104.0%,相对标准偏差不大于7.9%。结果表明,该方法能有效地减少蜂王浆中链霉素检测的假阳性结果,符合目前检测工作的需要。

A reliable and sensitive method was introduced for the analysis of streptomycin in royal jelly. The method was based on a separation by a C8 analytical column with β-naphthoquinone-4-sulfonate post-column derivatization and fluorescence detection. The clean-up of the extract was done by solid-phase extraction, firstly with an octadecyl cartridge and secondly with a cation-exchange cartridge. The linear range was 0.02-0.5 mg/L and the correlation coefficient was 0.995 8. The limits of detection （S/N=3） and quantitation （S/N=10） of streptomycin were 0.005 mg/kg and 0.01 mg/kg, respectively. The recoveries ranged from 84.0%to 104.0% with the relative standard deviations not larger than 7.9%. The method reduced the possibility of the false positive, and it could meet the need of the current work.