Simultaneous determination of propionic acid analgesic and antipyrtic drugs

建立了高效薄层色谱法测定镇痛、解热类药物的分析条件：薄层板;硅胶60 F254薄层板;溶剂系统;正丁基醚：正己烷：乙酸（20：4：1）;薄层板用0.1%二氯酚靛酚乙醇试剂喷雾后在100 ℃烘箱中加热10 min。除保泰松外，其余药物均呈淡红色或淡橙子，检出限为0.5- 5 μ g。用Liebermann试剂检测保泰松。以氯仿：甲醇：冰醋酸（45：5：1）为溶剂，用高效薄层色谱法分离了磺胺吡啶、对乙酰氨基酚和非那西丁。用茚三酮试剂检测磺胺吡啶。采用Liebermann试剂检测对乙酰氨基酚和非那西丁，建立了高效液相色谱法同时测定人血和尿中8种丙酸类镇痛解热药物的方法， ...更多信息 通过使用N-氯甲基邻苯二甲酰亚胺试剂在80 ° C下反应30分钟，以恒定产率合成了醛酰亚胺（MPI）衍生物。用C18键合相甲醇：水（70：30，v/v）为移动的流动相，在293 nm处对这些药物的MPI衍生物进行了分离和灵敏度测定。用Bond-Elut（C18）柱对人血和尿中的8种丙酸衍生物进行了萃取<encircledR>。用1.0ml乙腈：甲醇（80：20，v/v）对100 μ l血、尿样进行柱萃取，回收率为70- 100%。人血浆中丙酸类药物用氯仿在pH3.0条件下提取，用Bond Elut<encircledR>（硅胶）柱净化。采用柱上甲基化试剂（苯基三甲基氢氧化铵）对丙酸类药物的甲基衍生物进行气相色谱同时测定。丙酸类药物的甲基衍生物在5.0-25.0 μ g/ml范围内线性关系良好。甲基化药物的检测限为1.1-41.7ng。少

The analytical condition of analgesic and antipyretic drugs by HPTLC system was established as follows : plate ; silica gel 60 F254 HPTLC plate, solvent system ; n-butylether : n-hexane : acetic acid (20 : 4 : 1), detection method ; the plate was heated in oven at 100ﾟC for 10min after spraying with 0.1% dichlorophenolindophenol ethanol reagent. Pale red or pale orange color was given by these drugs except for phenylbutazone, and the detection limits were 0.5-5ug. Phenylbutazone was detected by the Liebermann reagent. Sulpyrine, acetaminophen and phenacetin showed satisfactory results of separation by HPTLC chromatogram using chloroform : methanol : acetic acid (45 : 5 : 1) as solvent system. Sulpyrine was detected by ninhydrin reagent. Acetaminophen and phenacetion were detected by Liebermann reagent.Simultaneously determination of eight propionic acid analgesic and antipyretic drugs in the human blood and urine was developed by HPLC.Propionic acid drugs were converted into methylphth … More alimide (MPI) derivatives with constant yield by reaction at 80ﾟC for 30min using a N-chloromethylphthalimide reagent. The MPI derivatives of these drugs showed satisfactory results of separation and sensitivity by HPLC using C18 bonded phase with methanol : water (70 : 30, v/v) as mobile phase at 293 nm. The extraction procedure of eight propionic acid derivatives added in the human blood and urine was performed with Bond-Elut^<<encircledR>> (C18) column. Yields of column extraction of 100 ul of blood and urine samples with 1.0 ml of acetonitrile : methanol (80 : 20, v/v) were 70-100%.A simultaneous determination of ten propionic acid analgesic and antipyretic drugs in human plasma was developed using a semiwide-bore capillary gas chromatography. The propionic acid drugs in human plasma were extracted with chloroform at pH 3.0, and were purified with Bond Elut<encircledR> (silica) column method. Methyl derivatives of propionic acid drugs by on-column methylation reagent (phenyltrimethylammonium hydroxide) were able to determine simultaneously by gas chromatography. Calibration curves of methyl derivatives of propionic acid drugs were linear at 5.0-25.0 ug/ml. The detection limits of the methylated drugs were ca 1.1-41.7ng oncolumn. Less