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目的建立犬血浆中盐酸右哌甲酯的UPLC-MS/MS检测方法。方法用甲基叔丁基醚提取犬血浆,离心后取上清液用氮气吹干,用甲醇-水(80∶20)溶解后进行质谱分析。采用BEH C18色谱柱(50 mm×2.1 mm,1.7μm),流动相为甲醇-0.2%甲酸(80∶20),流速0.1 mL·min-1,柱温45℃,进样量5μL。电喷雾离子化(ESI),正离子模式多重反应选择离子检测(MRM),盐酸右哌甲酯及卡马西平内标的检测离子对分别为m/z 234.33→84.56和237.35→194.31。结果盐酸右哌甲酯的线性范围为0.1～50 ng·mL-1(r=0.994,n=5),在犬血浆基质中,高、中、低浓度的日内、日间RSD均小于15%,方法的回收率为89%～103%,血浆基质对测定无干扰。结论所用方法处理简单、灵敏、特异性高,定量准确,为盐酸右哌甲酯制剂的临床药物动力学研究提供了简便、准确的分析测定方法。
Objective To establish a UPLC-MS / MS method for determination of right-methylphenidate hydrochloride in canine plasma. Methods The plasma of dog was extracted with methyl tert-butyl ether. After centrifugation, the supernatant was dried in nitrogen and dissolved in methanol-water (80:20) for mass spectrometry analysis. The mobile phase was methanol-0.2% formic acid (80:20) at a flow rate of 0.1 mL · min-1 using a BEH C18 column (50 mm × 2.1 mm, 1.7 μm) with a column temperature of 45 ° C and a sample volume of 5 μL. Electrospray ionization (ESI), positive ion mode multiple reaction selective ion detection (MRM), dexmedethanol hydrochloride and carbamazepine internal standard ion pairs were m / z 234.33 → 84.56 and 237.35 → 194.31 respectively. Results The linear range of right-methylphenidate hydrochloride was 0.1-50 ng · mL-1 (r = 0.994, n = 5). The intra-day and inter-day RSD of high, , The recovery rate of the method was 89% ~ 103%, no interference of plasma matrix on the determination. Conclusion The method is simple, sensitive, specific and accurate. It provides a simple and accurate method for the analysis of clinical pharmacokinetics of right-methylphenidate hydrochloride preparations.