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目的建立测定人血浆中莫西沙星浓度的HPLC法。方法以Kromasil C_8柱为色谱柱,含1%三乙胺的0.02 mol·L~(-1)磷酸二氢钾缓冲液(用磷酸调节pH至3.0):甲醇:乙腈(65:20:15,V/V/V)为流动相,流速1 mL·min~(-1),柱温30℃,检测波长296nm,进样量20μL,内标为加替沙星。血样以二氯甲烷提取,氮气流吹干后以流动相复溶进样。结果加替沙星、莫西沙星保留时间分别约为5.8、7.6 min,莫西沙星在血药浓度0.05～5.0 mg·L~(-1)内线性关系良好(r=0.999 8),最低定量限为0.05 mg·L~(-1),检测限0.015 mg·L~(-1)。方法回收率为99.37%～104.50%,提取回收率为80.48%～91.25%。日内精密度(RSD)为4.03%～5.73%,日间精密度(RSD)为4.53%～6.83%。样品在低温冷冻(-20℃)条件下至少3个月稳定。结论建立的HPLC法准确可靠,简便快速,灵敏度较高,可用于莫西沙星血药浓度测定及药动学研究。
Objective To establish an HPLC method for the determination of moxifloxacin in human plasma. Methods A Kromasil C_8 column was used as the mobile phase. 0.02 mol·L -1 potassium dihydrogen phosphate buffer containing 1% triethylamine adjusted to pH 3.0 with phosphoric acid: methanol: acetonitrile (65:20:15, V / V / V) as the mobile phase at a flow rate of 1 mL · min ~ (-1). The column temperature was 30 ℃, the detection wavelength was 296 nm, the injection volume was 20 μL and the internal standard was gatifloxacin. The blood sample was extracted with methylene chloride, and the sample was reconstituted with the mobile phase after the nitrogen stream was dried. Results The retention times of gatifloxacin and moxifloxacin were about 5.8 and 7.6 min, respectively. The moxifloxacin showed a good linear relationship (r = 0.999 8) at the plasma concentration of 0.05-5.0 mg · L -1, The limit of detection was 0.05 mg · L -1, and the limit of detection was 0.015 mg · L -1. The recoveries were 99.37% ~ 104.50% and the recovery rates were 80.48% ~ 91.25%. Intraday precision (RSD) was 4.03% ~ 5.73%, and daytime precision (RSD) was 4.53% ~ 6.83%. Samples are stable for at least 3 months at low temperature (-20 ° C). Conclusion The established HPLC method is accurate, reliable, simple, rapid and sensitive. It can be used for the determination of moxifloxacin and pharmacokinetics.