高效液相色谱-三重四极杆质谱法测定猪肉及肝脏中肾上腺素代谢物

Determination of metabolites of adrenaline in pork and liver by high performance liquid chromatography-triple quadrupole tandem mass spectrometry

目的建立高效液相色谱-三重四极杆质谱法同时测定猪肉及肝脏中2种肾上腺素代谢物4-羟基-3-甲氧基扁桃酸和3,4-二羟基扁桃酸。方法待测样品经含0.2%甲酸的乙腈-水混合溶液(80:20, V:V)提取、固相萃取柱净化,经ZORBAX SB-Aq色谱柱,用高效液相色谱-三重四极杆质谱仪进行测定。采用内标曲线法对目标化合物进行定量分析。结果本方法在线性范围2.5~120.0 ng/mL内,线性良好,相关系数为0.9999。方法检出限为0.3μg/kg,在低、中、高3个浓度下,样品加标回收率范围为60.2%~104.9%,相对标准偏差为1.3%~12.6%。结论本方法前处理简便,线性、回收率、灵敏度及重复性均满足方法学要求,可同时对猪肉及肝脏中的2种肾上腺素代谢物进行测定。

Objective To establish a method for simultaneous determination of 2 adrenaline metabolites, 4-hydroxy-3-methoxymandelic acid and 3,4-dihydroxymandelic acid, in pork and liver by high performance liquid chromatography-triple quadrupole tandem mass spectrometry(HPLC-MS). Methods Samples were extracted by 0.2% formic acid with acetonitrile-water(80:20, V:V), purified by solid phase extraction cartridges, separated by a ZORBAX SB-Aq column, and then detected by HPLC-MS. Internal standard curves were used for quantitative analysis. Results In the linear range of 2.5-120.0 ng/mL, the linear coefficient was 0.9999. The limit of detection was 0.3 μg/kg, and the recovery rates were 60.2%-104.9%, with relative standard deviation 1.3%-12.6%. Conclusion This method is simple, and the linear range, recovery, sensitivity and repeatability can meet the requirement of methodology. This method can be used for the simultaneous determination of 2 adrenaline metabolites in pork and liver.