LC-MS/MS法测定比格犬血浆中的阿那曲唑

用高效液相色谱-串联质谱法(LC-MS/MS)测定比格犬血浆中阿那曲唑的浓度。以苯磺酸氨氯地平为内标,加入50μL血浆,用甲基叔丁基醚萃取后取上清液以氮气吹干,用50%甲醇水溶液复溶,进样5μL,在电喷雾离子源下进行正离子检测。色谱柱为Agilent XDB C18(50mm×2.1mm×3.5μm),流动相为0.1%甲酸水-0.1%甲酸乙腈(60∶40)。阿那曲唑和内标的质荷比(m/z)分别为294.4和409,阿那曲唑和内标生成的主要碎片离子的质荷比(m/z)分别为255.3和238。阿那曲唑在0.5~500 ng·mL-1内线性良好,检出限为0.5ng·mL-1,提取回收率均大于80%,日内、日间准确度为101%~104%,日内、日间精密度分别小于7.04%和8.69%,已成功检测比格犬血浆中阿那曲唑的血药浓度。所用方法稳定、灵敏度好、分析时间短、提取回收率高,适用于比格犬血浆中阿那曲唑的血药浓度测定。

Determination of anastrozole in beagle dog plasma by LC-MS/MS

The HPLC-tandem mass spectrometry method （LC-MS/MS） was developed for the determination of anastrozole concentration in beagle dog plasma. 50 μL plasma samples were mixed with MTBE followed by extraction, the supernatant was dried under N2 and re-dissolved by 50% methanol, and 5 μL of which was injected onto LC-MS/MS. The analysis was carried out under the positive mode of electronic-spray ionization （ESI）. Chromatographic column was Agilent XDB C18 （50mm×2.1mm×3.5μm）, mobile phase was 0.1% formic acid in water-0.1% formic acid in acetonitrile （60：40）. The mass-to-charge ratio （m/z） of anastrozole and internal standard were 294.4-225.3 and 409-238, respectively. The linear range of anastrozole was within the concentration of 0.5-500 ng ·mL^-1. The LOD was 0.5 ng ·mL^-1. The extraction recoveries were all higher than 80%. The intra-and inter-day accuracy were 101%-104%, the intra-and inter-day precisions （RSD） were less than 7.04% and 8.69%, respectively. The anastrozole concentration in beagle dog plasma was detected successfully. The method was stable, sensitive, speedy and highly recovered. It was suitable for determining the anastrozole concentration in beagle dog plasma.