Zhejiang Province Key Laboratory of Mariculture & Enhancement, Zhejiang Marine Fisheries Research Institute, Zhoushan, China.
Anal Bioanal Chem. 2011 Aug;401(2):727-34. doi: 10.1007/s00216-011-5121-1. Epub 2011 Jun 3.
A rapid, specific, and sensitive method utilizing ultra-performance liquid chromatography tandem mass spectrometry was developed and validated to determine albendazole, albendazole sulfoxide, albendazole sulfone, and albendazole 2-aminosulfone in fish muscle tissue. The fish samples were extracted with ethyl acetate, then the organic phase was evaporated to dryness, and the residue was reconstituted in methanol-water solution and cleaned up by n-hexane. Reversed-phase separation of target compounds was achieved using a BEH C18 column and a gradient consisting of 0.2% (v/v) formic acid and methanol. Tandem mass spectrometry analyses were performed on a triple-quadrupole tandem mass spectrometer. In the whole procedure, the isotope-labeled internal standards were used to correct the matrix effect and variations associated with the analysis. The method was validated with respect to linearity, specificity, accuracy, and precision. The method exhibited a linear response from 0.1 to 20 ng mL(-1) (r(2) > 0.9985). The limit of quantitation for albendazole (ABZ), albendazole sulfoxide (ABZSO), albendazole sulfone (ABZSO(2)), and albendazole 2-aminosulfone (ABZ-2-NH(2)SO(2)) was 0.1, 0.1, 0.1, and 0.2 ng g(-1), respectively. The mean recoveries of ABZ, ABZSO, ABZSO(2), and ABZ-2-NH(2)SO(2) spiked at a level of 0.2-5.0 ng g(-1) were 95.3-113.7%, and the relative standard deviations of intra- and inter-day measurements were less than 6.38%. The method was later successfully applied to the determination of albendazole and its three metabolites in 60 fish samples collected from local markets.
建立并验证了一种利用超高效液相色谱串联质谱快速、特异、灵敏检测鱼肉组织中阿苯达唑、阿苯达唑砜、阿苯达唑亚砜和阿苯达唑 2-氨基砜的方法。鱼样用乙酸乙酯提取,有机相蒸干后用甲醇-水溶液复溶,再用正己烷萃取净化。目标化合物在 BEH C18 柱上以 0.2%(v/v)甲酸-甲醇梯度洗脱实现反相分离,串联质谱在三重四极杆串联质谱仪上进行分析。整个过程采用同位素内标校正基质效应和分析过程中的变化。方法进行了线性、专属性、准确度和精密度验证。该方法在 0.1-20ng mL(-1)(r(2) > 0.9985)范围内线性良好。阿苯达唑(ABZ)、阿苯达唑砜(ABZSO)、阿苯达唑亚砜(ABZSO(2))和阿苯达唑 2-氨基砜(ABZ-2-NH(2)SO(2))的定量下限分别为 0.1、0.1、0.1 和 0.2ng g(-1)。ABZ、ABZSO、ABZSO(2)和 ABZ-2-NH(2)SO(2)在 0.2-5.0ng g(-1)添加水平下的平均回收率为 95.3%-113.7%,日内和日间相对标准偏差均小于 6.38%。该方法成功应用于 60 个市售鱼肉样品中阿苯达唑及其三种代谢物的检测。