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目的建立大鼠血浆和脑组织中H102肽浓度测定的HPLC-ESI/MS法。方法血浆和脑组织样品采用甲醇沉淀蛋白后进样测定。色谱柱:Gemini C_(18)(50 mm×2.00mm,5μm),流动相:乙腈(0.1%甲酸)-水(0.1%甲酸)(14.5:85.5),流速0.4mL·min_(18),柱温40℃。采用电喷雾正离子模式离子化,选择m/z 645.3和m/z 843.2分别作为H102肽及内标安普利泰的检测离子。结果血浆及脑组织中H102肽在5~500μg·L~(-1)内线性良好(r=0.999 2,0.999 3);日内、日间精密度良好(RSD均<15%);提取回收率>85%。SD大鼠鼻腔给予H102肽溶液(2 mg·kg~(-1))后,主要药动学参数:t_(max)5 min,ρ_(max)103.13μg·L~(-1)。大鼠嗅球、大脑、小脑及海马中H102肽的AUC_(0→60min)分别为3 149.07、266.98、243.72及407.77μg·min·L~(-1)。结论本方法快速、准确、重复性好,适用于大鼠体内H102肽浓度的测定。
Objective To establish a HPLC-ESI / MS method for the determination of H102 peptide in rat plasma and brain. Methods Plasma and brain samples were assayed by methanol precipitation followed by injection. The mobile phase consisted of acetonitrile (0.1% formic acid) -water (0.1% formic acid) (14.5: 85.5) at a flow rate of 0.4 mL · min_ (18). The mobile phase consisted of Gemini C 18 (50 mm × 2.00 mm, Temperature 40 ℃. Electrospray positive ion mode ionization, m / z 645.3 and m / z 843.2, were chosen as the H102 peptide and the internal standard anpratrelate for detection. Results The H102 peptide in plasma and brain tissue showed a good linearity (r = 0.999, 2.09999) in the range of 5 ~ 500μg · L ~ (-1), the intra- and inter-day precision was good > 85%. After intranasal administration of H102 peptide solution (2 mg · kg -1), the main pharmacokinetic parameters were as follows: t max 5 min and max 103.13 μg · L -1. The AUC_ (0 → 60min) of H102 peptide in the olfactory bulb, brain, cerebellum and hippocampus were 3 149.07, 266.98, 243.72 and 407.77 μg · min · L -1, respectively. Conclusion The method is rapid, accurate and reproducible. It is suitable for the determination of H102 peptide in rats.