| 双柱固相萃取净化-液相色谱-串联质谱法测定牛奶和奶粉中链霉素和双氢链霉素残留量 |
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| 引用本文： | 刘晓茂,张进杰,张守军,曹亚平,杨志伟.双柱固相萃取净化-液相色谱-串联质谱法测定牛奶和奶粉中链霉素和双氢链霉素残留量[J].分析试验室,2010,29(10). |
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| 作者姓名： | 刘晓茂 张进杰 张守军 曹亚平 杨志伟 |
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| 作者单位： | 秦皇岛出入境检验检疫局,秦皇岛,066002 |
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| 摘 要： | 建立了双柱固相萃取净化-液相色谱-串联质谱(HPLC-MS/MS)测定牛奶和奶粉中链霉素和双氢链霉素残留量的分析方法。样品用H3PO4溶液提取,三氯乙酸沉淀蛋白,苯磺酸型和羧酸型固相萃取柱净化,经Atlantis C18色谱柱分离,以电喷雾离子源在正离子多反应监测(MRM)模式下进行测定。牛奶中链霉素和双氢链霉素的方法检出限均为4μg/kg,定量限均为10μg/kg,奶粉中链霉素和双氢链霉素的方法检出限均为30μg/kg,定量限均为80μg/kg,方法回收率为80%~86%,相对标准偏差为5.9%~11.5%。本方法适用于牛奶和奶粉中链霉素和双氢链霉素残留量的测定。
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| 关 键 词： | 液相色谱-串联质谱 双柱固相萃取净化 牛奶 奶粉 链霉素 双氢链霉素 残留 |
Determination of streptomycin and dihydrostreptomycin residues in milk and milk powder using dual solid-phase extraction clean up-liquid chromatography-tandem mass spectrometry |
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| HU Xiao-mao,ZHANG Jin-jie,ZHANG Shou-jun,CAO Ya-ping,YANG zhi-wei.Determination of streptomycin and dihydrostreptomycin residues in milk and milk powder using dual solid-phase extraction clean up-liquid chromatography-tandem mass spectrometry[J].Chinese Journal of Analysis Laboratory,2010,29(10). |
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| Authors: | HU Xiao-mao ZHANG Jin-jie ZHANG Shou-jun CAO Ya-ping YANG zhi-wei |
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| Institution: | LIU Xiao-mao,ZHANG Jin-jie,ZHANG Shou-jun,CAO Ya-ping and YANG zhi-wei (Qinhuangdao Entry-Exit Inspection and Quarantine Bureau,Qinhuangdao 066002) |
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| Abstract: | A method was developed for the determination of streptomycin and dihydrostreptomycin residues in milk and milk powder by dual solid-phase extraction clean up-liquid chromatography-tandem mass spectrometry(HPLC-MS/MS).The residues were extracted from the samples with phosphoric acid solutions,the proteins were precipitated by trichloroacetic acid and cleaned up with aromatic sulfonic acid and carboxylic acid solid phase extraction cartridge,then analyzed using HPLC-MS/MS in multiple reaction monitoring(MRM) ... |
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| Keywords: | Liquid Chromatography-tandem Mass Spectrometry(HPLC-MS/MS) Dual Solid-Phase Extraction Clean up Milk Milk powder Streptomycin Dihydrostreptomycin Residues |
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