RP-HPLC-UV法测定人血浆及痰液中的莫西沙星浓度

Determination of moxifloxacin in human plasma and sputum by RP-HPLC-UV

目的：建立反相高效液相色谱法以测定入血浆及痰液中莫西沙星浓度，用于比较莫西沙星在血浆及支气管分泌物的分布情况。方法：以乙腈沉淀血浆和痰液中的蛋白质，采用YMC C18色谱柱（150mm×4．6mm，5μm），柱温为室温，流动相为乙腈-0．01mol·L^-1磷酸二氢钾（22：78），磷酸二氢钾用磷酸调节pH值至2．70，流速为1．0mL·min～^-1。以乳酸环丙沙星为内标，检测波长为296nm。结果：血浆样品中的莫西沙星在0．0781～10mg·L^-1范围内线性关系良好（r=0．9956，w=1／C^2）；预处理回收率为90．45％～91．82％，方法回收率为96．91％～102．00％，日内RSD为1．17％～3．91％，日间RSD为1．84％～3．13％。痰液标本中的莫西沙星在0．1563～20mg·L^-1范围内线性关系良好（r=0．9913，W=1／C^2）；预处理回收率88．01％～91．78％，方法回收率85．12％～114．27％，日内RSD为1．70％～5．26％，日间RSD为2．48％～4．56％。结论：本方法快速、灵敏、准确、简便，适用于盐酸莫西沙星的血浆及痰液中的浓度测定。

Objective：To develop a RP-HPLC method for determining the concentration of moxifloxacin in human plasma and sputum. Methods：The protein in plasma and sputum was precipitated by aeetonitrile,and subsequently quantified by a RP-HPLC equipped with a YMC C18 column （150mm×4.6mm,5μm）. The samples were assayed at room temperature. The mobile phase consisted of aeetonitrile-0.01 mol·L^-1 potassium dihydrogen phosphate （22： 78, pH of buffer solution was adjusted to 2.70 by phosphoric acid）. Flow rate was 1.0 mL·min^-1. The detection wavelength was set at 296 nm. Ciprofloxaein was used as the internal standard. Results：The linearity of calibrated curves of plasma sample was in the range of 0.078 1 -10 mg·L^-1（r=0.9956,w =1/C^2）. The pretreatment recovery was 90.45% -91.82%The methodological recovery was 96.91% - 102.00%. The withinday RSDs were in the range of 1.17% -3.91% and inter-day RSDs of 1.84% -3.13%. The linearity of calibrated curves of sputum sample was in the range of 0. 156 3 -20 mg·L^-1（r = 0. 991 3,w = 1/C^2）. The pretreatment recovery was 88.01% -91.78%. The methodological recovery was 85. 12% -114.27%. The within-day RSDs were in the range of 1.70% -5.26% and inter-day RSDs of 2.48% -4.56%. Conclusion：The sensitive,accurate and easily manipulated assay offered a satisfactory tool for the pharmaeokineties and relative bioavailability of moxifloxacin in plasma and sputum samples.