孟娟,张晶,邵兵.超高压液相色谱-电喷雾串联四极杆质谱法测定猪肉食品中8种β-受体激动剂[J].食品安全质量检测学报,2013,4(1):129-134
超高压液相色谱-电喷雾串联四极杆质谱法测定猪肉食品中8种β-受体激动剂
Simultaneous determination of eight β-agonists residues in animal food by ultra pressure liquid chromatography-electrospray tandem mass spectrometry
投稿时间:2012-11-13  修订日期:2013-01-07
DOI:
中文关键词:  超高压液相色谱-串联质谱法  固相萃取  β-受体激动剂  食品安全  兽药残留
英文关键词:ultra pressure liquid chromatography-tandem mass spectrometry (UPLC-MS/MS)  solid- phase extraction  β-agonists  food safety  veterinary drugs residue
基金项目:国家高技术研究发展计划(863计划)项目(2010AA023001)、北京市卫生系统高层次卫生技术人才培养计划项目
作者单位
孟娟 北京疾病预防控制中心, 食物中毒诊断溯源技术北京市重点实验室 
张晶 北京疾病预防控制中心, 食物中毒诊断溯源技术北京市重点实验室 
邵兵 北京疾病预防控制中心, 食物中毒诊断溯源技术北京市重点实验室 
AuthorInstitution
MENG Juan Beijing Key Laboratory of Diagnostic and Traceability Technologies for Food Poisoning, Beijing Center for Disease Control and Prevention 
ZHANG Jing Beijing Key Laboratory of Diagnostic and Traceability Technologies for Food Poisoning, Beijing Center for Disease Control and Prevention 
SHAO Bing Beijing Key Laboratory of Diagnostic and Traceability Technologies for Food Poisoning, Beijing Center for Disease Control and Prevention 
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中文摘要:
      目的 采用超高压液相色谱-电喷雾串连四极杆质谱同时测定猪肉食品中8种β-受体激动剂残留。方法 试样中β-受体激动剂残留经酶解后超声提取, 低温离心后, 上清液用MCX固相萃取柱净化, Waters ACQUITY UPLCTM BEH C18色谱柱分离, 以甲醇?0.1%甲酸水溶液为流动相梯度洗脱, 最后用液相色谱-质谱/质谱进行测定。结果 该方法的平均回收率为75.6%~118.7%, 相对标准偏差小于25.0%, 方法的定量限为0.1~0.2 μg/kg。结论 该方法操作简单, 灵敏度高, 重现性良好, 适用于猪肉食品中β-受体激动剂残留的定性与定量检测。
英文摘要:
      Objective To develop an analytical method for the determination of eight kinds of β-agonists in animal producing food based on ultra pressure liquid chromatography-electrospray tandem mass spectrometry (UPLC-MS/MS). Methods Samples were enzymatic hydrolysed and extracted by acetic acid buffer (pH 5.2) and then purified and enriched by Oasis MCX solid phase extraction cartridges. The separation was performed on a Waters ACQUITY UPLCTM BEH C18 column (100 mm×2.1 mm i.d., 1.7 μm) with gradient elution using methanol and water containing 0.1% formic acid at a flow rate of 0.3 mL/min. Results Average recoveries of this method for fortified samples ranged from 75.6% to 118.7% with relative standard deviation less than 25.0%. The limits of quantitation (LOQ) for the whole method ranged from 0.1 μg/kg to 0.2 μg/kg. Conclusion Due to its high sensitivity and reproducibility, the method is suitable for the determination of agnoists in animal producing samples.
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