摘要
目的建立反相高效液相色谱法（RP-HPLC）测定脊柱结核患者患椎组织中异烟肼的浓度。方法色谱柱为Hypersil ODS C18（150am×4．6mm），以0．02mol／LKH2PO4（pH=4．0）-乙腈（70：30，V／V）为流动相，流速为1．0mL／min，检测波长为340nm。结果在0．024～0．75μg／g骨匀浆（相当于骨浓度0．24～7．5μg／g）范围内异烟肼峰面积与骨样本浓度呈良好线性关系（r=0．9993），提取回收率为82．69％～89．94％（n=5），方法回收率为97．60％～104．55％（n=5），13内、13间相对标准偏差分别为2．34％～4．28％，2．76％～5．83％（n=5）。结论本方法准确、精密度高、重复性好，是一种可靠的测定骨中异烟肼浓度的方法，适用于脊柱结核患者体内患椎骨组织中异烟肼浓度的定量分析，以便于判定和调整化疗方案以及指导手术病灶清除范围。
Objective A RP-HPLC method was developed for the determination of isoniazid in the vertebral focus of spinal tuberculosis. Methods The Hypersil BDS C18 chromatographic column （150 mm×4.6 mm）was used, and the mobile phase consisted of 0.02 mol/L phosphate buffer-acetonitrile （70：30, adjusted pH value to 4.0 with H3PO4 ） at a flow rate of 1.0 mL/min. Ultraviolet ray wavelength was 340 nm. Results Methodological evaluation showed when the bone homogenates concentration was from 0.024 μg/g to 0.750μg,/g（ equal to 0.24 to 7.50μg,/g in bone） , there was a good linear coefficient relation（ r = 0. 9993 ） between the peak area and the bone homogenates concentration（ r = 0.9993 ）. The extraction recovery was 82.69% to 89.94% （n =5）, the method recovery was 97, 60% to 104. 55% （n =5）, the within-day and between-day relative standard deviation were 2.34% to 4.28% and 2.76% to 5.83%, respectively （n = 5）. Conclusion The method is accurate, precise, and reproducible,which is suitable for the quantitative analysis of isonazid in veterbral focus and hence the further evaluation and adjustment of chemotherapeutic regimen as well as the directions of the focus＇ excision.
出处
《脊柱外科杂志》
2008年第3期165-168,190,共5页
Journal of Spinal Surgery
关键词
结核
脊柱
色谱法
液相
异烟肼
Tuberculosis, spinal
Chromatography, liquid
Isoniazid
