Chinese Journal of Chromatography

Chinese Journal of Chromatography ›› 2014, Vol. 32 ›› Issue (6): 566-572.DOI: 10.3724/SP.J.1123.2014.02009

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Determination of streptomycin and dihydrostreptomycin in pollens by high performance liquid chromatography-tandem mass spectrometry

HUANG Juan1,2, YIN Yao1, XU Jinzhong3, LIU Yan1, CHEN Guosong2, ZHANG Xiaoyan1, YANG Wenquan1, SHENG Chongyu1, CHEN Huilan1, ZHANG Rui1   

  1. 1. Animal, Plant and Food Inspection Center of Jiangsu Entry-Exit Inspection and Quarantine Bureau, Nanjing 210001, China;
    2. College of Science, Nanjing University of Technology, Nanjing 210009, China;
    3. Jiangsu Sinography Testing Co., Ltd., Nanjing 210061, China
  • Received:2014-02-17 Revised:2014-03-24 Online:2014-06-08 Published:2014-05-22

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Abstract:

A method was established for the determination of streptomycin (STR) and dihydrostreptomycin (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 matrices, 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.

Key words: dihydrostreptomycin, high performance liquid chromatography-tandem mass spectrometry (HPLC-MS/MS), pollens, solid phase extraction (SPE), streptomycin

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