| Project/Area Number |
07670505
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| Research Category |
Grant-in-Aid for Scientific Research (C)
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| Allocation Type | Single-year Grants |
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| Section | 一般 |
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| Research Field |
Legal medicine
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| Research Institution | KEIO UNIVERSITY |
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Principal Investigator |
SHINOZUKA Tatsuo Keio University, Legal Medicine, School of Medicine, Asistant Professor, 医学部・法医学, 講師 (70095610)
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| Co-Investigator(Kenkyū-buntansha) |
OGAMO Akira Kitasato University, Toxicology, School of Parmaceutical Sciences, Professor, 薬学部, 教授 (10050486)
YANAGIDA Junichi Keio University, Legal Medicine, School of Medicine, Professor, 医学部・法医学, 教授 (70049790)
KURODA Naohito Keio University, Legal Medicine, School of Medicine, Asistant Professor, 医学部・法医学, 講師 (40161799)
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| Project Period (FY) |
1995 – 1996
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| Project Status |
Completed (Fiscal Year 1996)
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| Budget Amount *help |
¥2,100,000 (Direct Cost: ¥2,100,000)
Fiscal Year 1996: ¥700,000 (Direct Cost: ¥700,000)
Fiscal Year 1995: ¥1,400,000 (Direct Cost: ¥1,400,000)
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| Keywords | Non-steroidal anti-inflammatory drugs (NSAID) / HPTLC / HPLC / GC / Analgesic drug |
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| Research Abstract |
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
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