色谱Issue(6)：566-572,7.DOI:10.3724/SP.J.1123.2014.02009
液相色谱-串联质谱法测定花粉中的链霉素和双氢链霉素
Determination of streptomycin and dihydrostreptomycin in pollens by high performance liquid chromatography-tandem mass spectrometry
摘要
Abstract
A method was established for the determination of streptomycin(STR)and dihydro-streptomycin(DHS)in pollens based on high performance liquid chromatography-tandem mass spectrometry(HPLC-MS / MS). The sample was extracted and cleaned-up by a C18 solid phase extraction cartridge. The separation was carried out on a Protemix WCX-NP5 column(100 mm ×2. 1 mm,5 μm)with a gradient elution using 5% ( v / v)formic acid,20 mmol / L ammonium acetate and methanol as mobile phases. The analysis of streptomycin and dihydrostreptomycin was performed under electrospray positive ionization mode. The limits of detection(LOD,S / N= 3)and limits of quantification( LOQ,S / N = 10)for the both were 5 μg / kg and 10 μg / kg, respectively. Good linearities(r ﹥0. 99)were achieved for the target compounds over the range of 10-200 μg / L. The recoveries at three spiked levels(10,20,50 μg / kg)in the blank matri-ces,such as pollen pini,corn pollen,camellia pollen,sunflower pollen,rape pollen and bee pollen,were from 76. 8% to 100. 3% with the relative standard deviations varied from 3. 70% to 12. 6% . The method is accurate,practical,and can be applied to most of the contaminated matrices. With this method,heptafluorobutyric acid is not required as mobile phase which is harmful to MS spectrometer.关键词
固相萃取/高效液相色谱-串联质谱/链霉素/双氢链霉素/花粉Key words
solid phase extraction( SPE)/high performance liquid chromatography-tandem mass spectrometry(HPLC-MS / MS)/streptomycin/dihydrostreptomycin/pollens分类
化学化工引用本文复制引用
黄娟,张睿,殷耀,徐锦忠,刘艳,陈国松,张晓燕,杨雯筌,沈崇钰,陈惠兰..液相色谱-串联质谱法测定花粉中的链霉素和双氢链霉素[J].色谱,2014,(6):566-572,7.基金项目
质检公益项目（200810099）；质检 SN 行业标准制订项目（2011B288K）． （）
