论文部分内容阅读
目的建立测定人血清和脑脊液中莫西沙星药物浓度的高效液相色谱方法。方法血清和脑脊液取样量均为10μL;采用Shima-pack CLC-ODS色谱柱(6.0 mm×150 mm,5μm)进行分离;以0.01 mol.L-1磷酸缓冲液(含硫酸四丁基铵5mmol.L-1,pH 2.5)-乙腈(80∶20)为流动相;吡哌酸为内标,荧光检测器波长:Ex=295 nm、Em=495 nm。结果内标和莫西沙星的保留时间分别为2.93和6.39 min;血清和脑脊液标准曲线在0.2～20 mg.L-1内线性良好(r>0.999 9,n=5),其高、中、低质控样本方法学回收率分别在98.08%～104.81%和92.08%～101.73%间,方法学误差批内RSD均小于5.5%,批间RSD均小于7.8%。扩大取样量至0.1 mL,标准曲线下限可达2 ng.mL-1并良好检出。结论该方法取样量小、操作简便、灵敏度高;为进行血清和脑脊液中莫西沙星临床PK/PD研究提供了数据保障。
Objective To establish a high performance liquid chromatographic method for the determination of moxifloxacin in human serum and cerebrospinal fluid. Methods Serum and cerebrospinal fluid (CSF) samples were all collected in a volume of 10 μL. Shima-pack CLC-ODS column (6.0 mm × 150 mm, 5 μm) was used for the separation. 0.01 mol·L-1 phosphate buffer L-1, pH 2.5) -acetonitrile (80:20) as mobile phase and pipemidic acid as internal standard. The fluorescence detector wavelength was 295 nm for Ex = 495 nm. Results The retention time of internal standard and moxifloxacin were 2.93 and 6.39 min, respectively. The standard curve of serum and cerebrospinal fluid was linear within 0.2 ~ 20 mg.L-1 (r> 0.999 9, n = 5) The methodological recoveries of low-quality control samples ranged from 98.08% to 104.81% and from 92.08% to 101.73%, respectively. The RSDs within the methodological error batch were less than 5.5%, and the inter-item RSDs were less than 7.8%. Expand the sampling volume to 0.1 mL with a lower limit of the standard curve of 2 ng.mL-1 and good detection. Conclusions This method is simple in sampling, simple in operation and high in sensitivity. It provides a data guarantee for clinical PK / PD study of moxifloxacin in serum and cerebrospinal fluid.