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快速高分离液相色谱-串联质谱法检测原乳中活性β-内酰胺酶
引用本文:孙汉文,李挥,张敬轩,周正.快速高分离液相色谱-串联质谱法检测原乳中活性β-内酰胺酶[J].分析化学,2010,38(8).
作者姓名:孙汉文  李挥  张敬轩  周正
作者单位:1. 河北省分析科学重点实验室,河北大学化学与环境科学学院,保定,071002
2. 河北省分析科学重点实验室,河北大学化学与环境科学学院,保定,071002;河北省食品质量监督检验研究院,石家庄,050051
3. 河北省食品质量监督检验研究院,石家庄,050051
基金项目:河北省科技支撑项目基金 
摘    要:建立了原乳中活性β-内酰胺酶拮抗剂的快速高分离液相色谱-串联质谱(RRLC-MS/MS)检测方法.利用活性β-内酰胺酶能够酶解青霉素族药物的特性,在原乳中加入适量氨苄青霉素,酶解1 h后,检测原乳中氨苄青霉素酶解率,定性检测活性目标物.试样中氨苄青霉素经乙腈溶液提取,HLB固相萃取柱净化和浓缩后,RRLC-MS/MS多反应监测模式定性与定量分析.本方法对活性β-内酰胺酶检出限为4 U/mL;对原乳中添加1 mg/kg水平氨苄青霉素的加标回收率为92.3%~95.5%;相对标准偏差RSD≤10%(n=6).本方法的定性结果与生物杯碟法完全一致.

关 键 词:液相色谱-串联质谱  原乳  β-内酰胺酶

Qualitative Analysis of Active Beta-Lactamases in Milk Samples by Rapid Resolution Liquid Chromatography-Tandem Mass Spectrometry
SUN Han-Wen,LI Hui,ZHANG Jing-Xuan,ZHOU Zheng.Qualitative Analysis of Active Beta-Lactamases in Milk Samples by Rapid Resolution Liquid Chromatography-Tandem Mass Spectrometry[J].Chinese Journal of Analytical Chemistry,2010,38(8).
Authors:SUN Han-Wen  LI Hui  ZHANG Jing-Xuan  ZHOU Zheng
Institution:SUN Han-Wen1,LI Hui1,2,ZHANG Jing-Xuan2,ZHOU Zheng2 1(Key Laboratory of Analytical Science of Hebei,College of Chemistry and Environmental Science,Hebei University,Baoding 071002) 2(Hebei Institute of Food Quality Supervision Inspection and Research,Shijiazhuang 050051)
Abstract:A rapid resolution liquid chromatography-tandem mass spectrometric method (RRLC-MS/MS) has been developed for the qualitative analysis of active beta-lactamases in milk samples. Penicillin was added to the samples solution to enzymolyze the active beta-lactamases. Then,the analytes were extracted by CH3CN-H2O from homogenized samples,and the extract was cleaned by Oasis HLB solid phase extraction cartridge. Quantification of penicillin was achieved by RRLC-MS/MS with multiple reaction monitoring. Detection ...
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