Abstract:The aim of this study was to establish a UPLC-MS/MS method for rapid determination of five β-agonists in pork liver, beef and mutton. The five β-agonists in samples were extracted with 80% acetonitrile, purified by PRiME HLB solid phase extraction column, concentrated by nitrogen, and finally dissolved with 10% methanol. A gradient elution was performed using 10 mmol/L ammonium acetate aqueous solution-10 mmol/L ammonium acetate methanol (pH=5) as a mobile phase. The multi-reaction monitoring (MRM) mode was used for the determination, and internal standard method was used for quantification. The concentration of five β-agonists showed good linearity in the range of 0.5 to 50.0 ng/mL with the coefficient correlation (R2) between 0.999 63 to 0.999 96. At the standard addition levels of 0.5, 1.0 and 5.0 μg/kg, the average recovery ratio of five β-agonists was 93.7% to 106.1% in pork liver, 95.2% to 104.0% in beef, and 95.1% to 106.0% in mutton. The test indicated that the method showed good accuracy and repeatability. Based on S/N=3, the detection limit of five β-agonists was 0.01 to 0.04 μg/kg, and quantitation limit was 0.02 to 0.15 μg/kg. This method is simple, sensitive, accurate, and suitable for large quantities animal products detection analysis.
张苏珍, 王益军, 田蕴, 贺燕, 葛敏. 猪肝、牛肉、羊肉中5种β-受体激动剂残留的超高效液相色谱-串联质谱分析方法的建立[J]. 动物营养学报, 2018, 30(10): 4087-4094.
ZHANG Suzhen, WANG Yijun, TIAN Yun, HE Yan, GE Min. UPLC-MS/MS Method for the Determination of Five β-agonists Residue in Pork Liver, Beef and Mutton. Chinese Journal of Animal Nutrition, 2018, 30(10): 4087-4094.
WANG P L,LIU X M,SU X O,et al.Sensitive detection of β-agonists in pork tissue with novel molecularly imprinted polymer extraction followed liquid chromatography coupled tandem mass spectrometry detection[J].Food Chemistry,2015,184:72-79.
[13]
PAN S D,ZHOU L X,ZHAO Y G,et al.Development and validation of a sensitive method for simultaneous determination of eight β2-agonists in pork by ultrasonic-assisted extraction and liquid chromatography/tandem mass spectrometry[J].Chromatographic Science,2015,53(1):104-111.
[14]
SUNG I K,PARK S J,KANG K,et al.Development and application of a method for rapid and simultaneous determination of three β-agonists (clenbuterol,ractopamine,and zilpaterol) using liquid chromatography-tandem mass spectrometry[J].Korean Journal for Food Science of Animal Resources,2015,35(1):121-129.
MAURO D,CIARDULLO S,CIVITAREALE C,et al.Development and validation of a multi-residue method for determination of 18β-agonists in bovine urine by UPLC-MS/MS[J].Microchemical Journal,2014,115:70-77.
[4]
COURTHEYN D,LE BIZEC B,BRAMBILLA G,et al.Recent developments in the use and abuse of growth promoters[J].Analytica Chimica Acta,2002,473(1/2):71-82.