色谱

色谱

• 技术与应用 • 上一篇    下一篇

高效液相色谱柱后衍生法测定蜂王浆中的链霉素

张晓燕1,徐锦忠1,2,沈崇钰1,陈惠兰1,吴斌1

  

  1. 1.Animal, Plant and Food Inspection Center (APFIC) of Jiangsu Entry-Exit Inspection and
    Quarantine Bureau, National Honey Reference Laboratory, Nanjing 210001, China;
    2.Jiangsu Engineering Research Center for Apiculture, Nanjing 211800, China
  • 收稿日期:2007-09-25 修回日期:2007-12-17 出版日期:2008-05-30 发布日期:1984-03-25
  • 通讯作者: 徐锦忠

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

ZHANG Xiaoyan1, XU Jinzhong1,2, SHEN Chongyu1, CHEN Huilan1, WU Bin1   

  1. 1.Animal, Plant and Food Inspection Center (APFIC) of Jiangsu Entry-Exit Inspection and
    Quarantine Bureau, National Honey Reference Laboratory, Nanjing 210001, China;
    2.Jiangsu Engineering Research Center for Apiculture, Nanjing 211800, China
  • Received:2007-09-25 Revised:2007-12-17 Online:2008-05-30 Published:1984-03-25
  • Contact: XU Jinzhong1

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摘要：

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0.01 mol/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0.02～0.5 mg/L,相关系数为0.9958,方法的检出限和定量限分别为为
0.005 mg/kg和0.01 mg/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。

关键词: 蜂王浆 , 高效液相色谱法, 链霉素, 柱后衍生

Abstract:

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 0.9958. 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.

Key words: post-column derivatization, royal jelly
, streptomycin, high performance liquid chromatography (HPLC)