色谱

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

• 研究论文 • 上一篇    下一篇

液相色谱-串联质谱法测定花粉中的链霉素和双氢链霉素

黄娟1,2, 殷耀1, 徐锦忠3, 刘艳1, 陈国松2, 张晓燕1, 杨雯筌1, 沈崇钰1, 陈惠兰1, 张睿1   

  1. 1. 江苏出入境检验检疫局动植物与食品检测中心, 江苏 南京 210001;
    2. 南京工业大学理学院, 江苏 南京 210009;
    3. 江苏中谱检测有限公司, 江苏 南京 210061
  • 收稿日期:2014-02-17 修回日期:2014-03-24 出版日期:2014-06-08 发布日期:2014-05-22
  • 通讯作者: 黄娟
  • 基金资助:

    质检公益项目（200810099）；质检SN行业标准制订项目（2011B288K）.

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

PDF

442

被引次数

23

摘要：

建立了花粉中链霉素（streptomycin，STR）与双氢链霉素（dihydrostreptomycin，DHS）的高效液相色谱-串联质谱（HPLC-MS/MS）检测方法。样品经提取液提取、三氯甲烷沉淀蛋白后，用C18固相萃取柱进行富集净化，采用HPLC-MS/MS对目标物进行定性确证和定量分析。在Protemix WCX-NP5色谱柱（100 mm×2.1 mm，5 μm）上以5%（v/v）甲酸、20 mmol/L醋酸铵和甲醇为流动相进行梯度洗脱分离；质谱采集模式为电喷雾正离子监测模式。链霉素和双氢链霉素的检出限（以信噪比（S/N）=3计）均为5 μg/kg，定量限（以S/N=10计）均为10 μg/kg；在10~200 μg/L的质量浓度范围内呈现良好的线性关系，相关系数（r）大于0.99。本底空白的松花粉、玉米花粉、茶花粉、葵花粉、油菜花粉、杂花粉等6种基质中10、20、50 μg/kg添加水平下的加标回收率范围为76.8%~100.3%，精密度范围为3.70%~12.6%。该方法无需使用对LC-MS联用仪容易造成污染的七氟正丁酸，且方法准确可靠，适用于大部分花粉基质的测定。

关键词: 高效液相色谱-串联质谱, 固相萃取, 花粉, 链霉素, 双氢链霉素

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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