Yu Donglei, Rummel Nathan, Shaikh Badar
U.S. Food and Drug Administration, Center for Veterinary Medicine, Office of Research, 8401 Muirkirk Rd, Laurel, MD 20708, USA.
J AOAC Int. 2011 Mar-Apr;94(2):446-52.
An HPLC method was developed for the determination of albendazole (ABZ) and its metabolites, a sulfoxide (ABZSO), a sulfone (ABZSO2), and albendazole-2-aminosulfone (ABZ-2-NH2SO2), from yellow perch muscle tissue with adhering skin. The muscle tissue samples were made alkaline with potassium carbonate and extracted with ethyl acetate, followed by a series of liquid-liquid extraction steps. After solvent evaporation, the residue was reconstituted in the initial mobile phase combination of the gradient. The mobile phase consisted of a buffer, 50 mM ammonium acetate (pH = 4.0) in 10% methanol-water, and 100% acetonitrile. The gradient was from 20% acetonitrile to 85% acetonitrile. The analytes were chromatographed on an RP Luna C18(2) column and detected by fluorescence with excitation and emission wavelengths of 290 and 330 nm, respectively. The average recoveries from fortified muscle tissue for ABZ (20-100 ppb), ABZ-SO (20-200 ppb), ABZSO2 (8-100 ppb), and ABZ-2-NH2SO2 (20-100 ppb) were 85, 95, 101, and 86%, respectively, with corresponding CV values of 9, 3, 6, and 4%, respectively. Their LOQ values were 10, 10, 1, and 10 ppb, respectively. The procedure was applied to determine ABZ and its major metabolites in the incurred muscle tissue of yellow perch obtained after orally dosing the fish with ABZ.
建立了一种高效液相色谱法,用于测定带皮黄鲈肌肉组织中的阿苯达唑(ABZ)及其代谢产物亚砜(ABZSO)、砜(ABZSO2)和阿苯达唑-2-氨基砜(ABZ-2-NH2SO2)。肌肉组织样品用碳酸钾碱化,用乙酸乙酯萃取,然后进行一系列液-液萃取步骤。溶剂蒸发后,残留物用梯度初始流动相组合复溶。流动相由缓冲液、10%甲醇-水的50 mM乙酸铵(pH = 4.0)和100%乙腈组成。梯度为从20%乙腈到85%乙腈。分析物在RP Luna C18(2)柱上进行色谱分离,并用荧光检测,激发波长和发射波长分别为290和330 nm。在添加了ABZ(20-100 ppb)、ABZ-SO(20-200 ppb)、ABZSO2(8-100 ppb)和ABZ-2-NH2SO2(20-100 ppb)的强化肌肉组织中的平均回收率分别为85%、95%、101%和86%,相应的CV值分别为9%、3%、6%和4%。它们的定量限分别为10 ppb、10 ppb、1 ppb和10 ppb。该方法用于测定用ABZ口服给药后获得的黄鲈肌肉组织中ABZ及其主要代谢产物。