摘要
目的 :建立生物样品中甲氨喋呤 (MTX)浓度测定方法。方法 :固相萃取净化和富集样品 ,高效液相色谱法测定血清和脑脊液中MTX含量。色谱条件 :以C18柱为分析柱 ,流动相为甲醇 -乙腈 -磷酸盐缓冲液 (2∶7∶91) ,流速 0 8mL·min-1,柱温 2 5℃ ,检测波长 313nm。结果 :在 0 0 5～ 80 μg·mL-1范围内呈线性 ,回收率为 90 %以上 ,血清中MTX最低检测限为 10ng·mL-1,脑脊液中最低检测限为 5ng·mL-1。结论 :本法简便、快速、灵敏度高、特异性强 ,适合于生物样品中MTX监测及药物动力学研究。
Objective:Determination of the content of methotrexate(MTX) in serum or cerebrospinal fluid was reported.Method:0\^5 mL serum or 1 mL cerebrospinal fluid (CFS) sample was loaded on to the Spe column, subsequently,the column was washed with 3 mL 0\^9% NaCl injection,to remove serum or CFS proteins and contaminants.The free MTX which remained bound to the column was then eluted with 2 mL of methanol.The methanol fraction was dried at 60 ℃ under a jet of nitrogen,and then dissolved in methanol-water(50∶50).20 μL sample was injected into the chromatograph.The C 18 reversed phase column was used,mobile phase:methanol-acetonitrile-phosphate buffer solution(pH 5 8) (2∶7∶91),flow rate 0\^8 mL·min -1 ,column temperature 25 ℃, the detection was carried out with an ultraviolet detector at 313 nm.Results:The linearity was in the range of 0\^05～80 μg·mL -1 .The absolute recoveries of MTX both in serum and CFS were up to 90\^0%.The detection limit of MTX in serum and CFS were respectively 10 ng·mL -1 and 5 ng·mL -1 .Any interferent peaks from commonly chemotherapeutants weren′t found.Conclusion:This paper provides a rapid,convenient,sensitive and accurate method suitable for monitoring and pharmacokinetics study of MTX.
出处
《药物分析杂志》
CAS
CSCD
北大核心
2000年第6期401-404,共4页
Chinese Journal of Pharmaceutical Analysis
