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0.1~0.2μg/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.
Objective To develop an analytical method for the determination of eight kinds ofβ-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., 1.7μm) 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.
出处
《食品安全质量检测学报》
CAS
2013年第1期129-134,共6页
Journal of Food Safety and Quality
基金
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~~
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
ultra pressure liquid chromatography-tandem mass spectrometry (UPLC-MS/MS)
solidphase extraction
β-agonists
food safety
veterinary drugs residue
