中国临床药学杂志

目的建立测定血浆、肺组织、支气管黏膜、肺泡灌洗液和痰液中左氧氟沙星浓度的方法。方法固定相为TSK-gelODS-80TM C18柱(150 mm×4.6 mm,5μm);流动相为50 mmol.L-1KH2PO4(pH 2.0)四氢呋喃-1 mol.L-1醋酸铵(92/7/1,V/V/V);荧光检测波长Ex/Em为296/504 nm,流速1.0 mL.min-1。结果各质控浓度的血浆、肺组织、支气管黏膜、肺泡灌洗液和痰液中左氧氟沙星的萃取回收率分别为94.2%~98.4%、100.2%~103.7%、99.3%~100.5%、99.9%~102.2%和100.6%~100.9%。各质控浓度的血浆、肺泡灌洗液、痰液和缓冲液测定结果日内RSD分别≤3.6%、≤5.3%、≤5.2%和≤1.7%,方法回收率分别为91.5%~110%、96.7%~100.5%、99.5%~103.8%和96.3%~103%;日间RSD分别≤3.5%、≤6.3%、≤6.3%和≤4.1%。血浆、肺泡灌洗液、痰液和缓冲液中左氧氟沙星质量浓度为0.01⁵.00 mg.L-1时具有良好的线性关系(r=0.999 6⁰.999 9)。左氧氟沙星在上述组织体液中最低检测限浓度为0.01 mg.L-1。结论本试验建立的HPLC方法灵敏准确、特异性高,可用于测定血浆、肺组织、支气管黏膜、肺泡灌洗液和痰液中左氧氟沙星的浓度。

AIM To establish the high performance liquid chromatography(HPLC) method for determination of the concentration of levofloxacin in plasma,lung,bronchus membrane,bronchoalveolar lavage fluid(BALF) and sputum.METHODS The HPLC was performed on TSK-gel ODS-80TM C18(150 mm×4.6 mm,5 μm) column.The mobile phase consisted of 50 mmol·L-1 KH2PO4(pH 2.0)-tetrahydrofuran-1 mol·L-1 CH3COONH4(92/7/1,V/V/V).The detection wavelength(Ex/Em)was set at 296 nm/504 nm.The flow rate was 1.0 mL·min-1.RESULTS The extraction recovery of each quality control concentration of plasma,lung,bronchus membrane,BALF and sputum was 94.2%-98.4%,100.2%-103.7%,99.3%-100.5%,99.9%-102.2% and 100.6%-100.9%,respectively.The inter-day coefficient variation of each quality control concentration of plasma,BALF,sputum and buffer was less than 3.6%,5.3%,5.2% and 1.7%,respectively.The method recovery was 91.5%-110%,96.7%-100.5%,99.5%-103.8% and 96.3%-103%,respectively.The intra-day coefficient variation was less than 3.5%,6.3%,6.3% and 4.1%,respectively.A good linearity was shown in the concentration range 0.01-5.00 mg·L-1 for all constituents(r=0.999 6-0.999 9).The minimum detection limit concentration of levofloxacin in above tissues and body fluids was 0.01 mg·L-1.CONCLUSION The method of establishment is sensitive,accurate and has a high specificity.It is a suitable method for determining the drug concentration of levofloxacin in plasma,lung,bronchus membrane,BALF and sputum.