色谱

色谱 ›› 2012, Vol. 30 ›› Issue (01): 33-38.DOI: 10.3724/SP.J.1123.2011.08009

• 研究论文 • 上一篇    下一篇

串联双柱固相萃取-液相色谱-串联质谱法测定番茄酱中链霉素和双氢链霉素残留量

巩志国1, 苏敏1, 季新成1*, 李世雨1, 万宇平2   

  1. 1. 新疆出入境检验检疫局技术中心, 新疆 乌鲁木齐 830063; 2. 北京望尔生物技术有限公司, 北京 102206
  • 收稿日期:2011-08-04 修回日期:2011-10-14 出版日期:2012-01-28 发布日期:2012-03-01
  • 通讯作者: 季新成,博士,工程师,主要从事进出口食品检测技术研究. Tel: (0991)4640279,
  • 基金资助:
    新疆出入境检验检疫局科研项目(No. 2010xk0048).

Determination of streptomycin and dihydrostreptomycin residues in tomato paste by tandem dual solid phase extraction column-liquid chromatography-tandem mass spectrometry

GONG Zhiguo1, SU Min1, JI Xincheng1*, LI Shiyu1, WAN Yuping2   

  1. 1. Technique Center of Xinjiang Entry-Exit Inspection and Quarantine Bureau, Urumqi 830063, China; 2. Beijing Wanger Biotechnology Co., Ltd., Beijing 102206, China
  • Received:2011-08-04 Revised:2011-10-14 Online:2012-01-28 Published:2012-03-01

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386

被引次数

19

摘要： 建立了同时测定番茄酱中链霉素和双氢链霉素残留量的串联双柱净化-液相色谱-串联质谱方法。样品中的残留物用磷酸盐缓冲液(pH 4)提取,经分散固相萃取净化和串联双柱固相萃取净化后,用极性色谱柱在梯度洗脱条件下分离待测物,采用正离子电喷雾离子源(ESI+)在多反应监测(MRM)扫描模式下进行测定,外标法定量。链霉素和双氢链霉素在0.01～0.2 mg/L质量浓度范围内线性关系良好,相关系数(r)大于0.999。链霉素和双氢链霉素的定量限均为0.02 mg/kg,回收率为71%～101%,相对标准偏差为2.3%～15%。该方法操作简便,净化效果好,灵敏,准确,适用于检测和分析番茄酱及其制品中链霉素和双氢链霉素残留量。

关键词: 串联双柱固相萃取净化, 番茄酱, 链霉素, 双氢链霉素, 液相色谱-串联质谱

Abstract: The method was specifically developed for the simultaneous determination of streptomycin and dihydrostreptomycin residues in tomato paste by tandem dual solid phase extraction (SPE) column cleanup-liquid chromatography-tandem mass spectrometry. The residues were extracted from the samples with phosphate buffer solution (pH 4). The cleanup was performed by the way of dispersive solid phase extraction and tandem dual solid phase extraction column. The polar chromatographic column was used to complete the separation of the analytes under gradient elution and the analytes were detected in multiple reaction monitoring (MRM) mode via positive electrospray ionization (ESI+). The external standard calibration curves were used for the quantification. The linear ranges were from 0.01 to 0.2 mg/L with a good linear relationship (r＞0.999) for streptomycin and dihydrostreptomycin. The limit of quantification (LOQs) was 0.02 mg/kg for the both analytes. The recovery range was from 71% to 101% with the relative standard deviations (RSDs) between 2.3% and 15%. It was indicated that this method is accurate, easier, more sensitive, and has a better purification effect in the monitoring and analysis. The method is accurate and specific to monitor and analyze of streptomycin and dihydrostreptomycin residues in tomato paste and its products.

Key words: dihydrostreptomycin, liquid chromatography-tandem mass spectrometry (LC-MS/MS), streptomycin, tomato paste, tandem dual solid phase extraction column cleanup