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

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

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.