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串联双固相萃取柱-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

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

作者信息

Gong Zhiguo, Su Min, Ji Xincheng, Li Shiyu, Wan Yuping

机构信息

Technique Center of Xinjiang Entry-Exit Inspection and Quarantine Bureau, Urumqi 830063, China.

出版信息

Se Pu. 2012 Jan;30(1):33-8. doi: 10.3724/sp.j.1123.2011.08009.

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.

摘要

该方法是专门为通过串联双固相萃取(SPE)柱净化-液相色谱-串联质谱法同时测定番茄酱中链霉素和双氢链霉素残留量而开发的。用磷酸盐缓冲溶液(pH 4)从样品中提取残留量。通过分散固相萃取和串联双固相萃取柱的方式进行净化。使用极性色谱柱在梯度洗脱条件下完成分析物的分离,并通过正电喷雾电离(ESI +)在多反应监测(MRM)模式下检测分析物。采用外标校准曲线进行定量。链霉素和双氢链霉素的线性范围为0.01至0.2 mg/L,具有良好的线性关系(r>0.999)。两种分析物的定量限(LOQ)均为0.02 mg/kg。回收率范围为71%至101%,相对标准偏差(RSD)在2.3%至15%之间。结果表明,该方法在监测分析中准确、简便、灵敏,净化效果较好。该方法对于监测和分析番茄酱及其制品中链霉素和双氢链霉素残留量准确且具有特异性。

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