1.Analysis of primary metabolites of alpha-tocopherol in human urine by liquid chromatography-mass spectrometry.
Ying-Yu PAN ; Ying YU ; Gu-Xian LAI ; Li-Cai ZHU
Acta Pharmaceutica Sinica 2008;43(6):634-639
To investigate primary metabolites of alpha-tocopherol in human urine, the urine samples of five healthy volunteers after oral administration of 250 mg vitamin E once a day for seven days were collected within 0 -6 h in the seventh day. The samples were purified through C18 solid-phase extraction cartridge and analyzed by liquid chromatography-tandem mass spectrometry. alpha-Tocopheronic acid, 2,5,7, 8-tetramethyl-2-(2'-carboxyethyl) -6-suphate-chroman (alpha-CEHC-sulphate), gamma-tocopheronolactone, and 2, 5, 7, 8-tetramethyl-2-(4', 8', 12'-trimethyl-12'-carboxy dodecanyl) -6-suphate-chroman were found in urine of volunteers as four primary metabolites of alpha-tocopherol. The method has shown to be promising for alpha-tocopherol detection with many desirable properties including high sensitivity and selectivity, thus providing a reliable pathway for further study in metabolism of alpha-tocopherol.
Administration, Oral
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Antioxidants
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administration & dosage
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pharmacokinetics
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Chromatography, High Pressure Liquid
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methods
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Humans
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Spectrometry, Mass, Electrospray Ionization
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methods
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Vitamin E
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pharmacokinetics
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alpha-Tocopherol
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metabolism
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urine
2.Studies on quality standard of Yifu ointment.
You-ming PU ; Yi ZHANG ; Rui GU ; Xian-rong LAI ; Juan DU ; Ren-chao LI
China Journal of Chinese Materia Medica 2007;32(22):2368-2370
OBJECTIVETo develop a method for the determination of Chonglou saponin I and Chonglou saponin II in Yifu ointment.
METHODThe chromatographic separation was performed on Hypersil ODS2 C18 column (4.6 mm x 150 mm, 5 microm) and IBBM-612111 ODS C18 guard column. Acetonitrile-0.02% phosphoric (43:57) as mobile phase. The flow rate was 1 mL min(-1) and column temperature was set at 40 degrees C. The UV detection wavelength was set 203 nm.
RESULTChonglou saponin I showed a good linear relationship at a range of 0.1024-3.2 microg, r =0.9998, the average recovery was 97.4%, and RSD was 1.8% (n = 6); Chonglou saponin II showed a good linear relationship at a range of 0.064-2.0 microg, r = 0.9999, the average recovery was 101.4%, and RSD was 1.0% (n =6).
CONCLUSIONThe method is accurate with the good reproducibility and can be used for the quality control of Yifu Ointment.
Chromatography, High Pressure Liquid ; Drug Combinations ; Drugs, Chinese Herbal ; chemistry ; isolation & purification ; standards ; Liliaceae ; chemistry ; Ointments ; Plants, Medicinal ; chemistry ; Quality Control ; Reproducibility of Results ; Rosaceae ; chemistry ; Saponins ; analysis
3.Quality standard for Xindi soft capsule.
Yu-Jie WANG ; Yi ZHANG ; Rui GU ; Xian-Rong LAI ; Ping WANG ; Zhu-Jun ZHANG
China Journal of Chinese Materia Medica 2006;31(7):552-597
OBJECTIVETo establish the quality control standard of Xindi soft capsule.
METHODQuercetin, kaempferol and isorhamnetin were isolated by TLC with chloroform-ethyl formate-formic acid (5:4:1). The chromatographic separation was performed on a Diamonsil C18 column (4.6 mm x 250 mm, 5 microm). Acetonitrile-water-phosphoric (30:70:0.1) as mobile phase. The flow rate was 1 mL x min(-1) and column temperature was set at 40 degrees C. The UV detection wavelength was set at 254 nm.
RESULTQuercetin, Kaempferol and Isorhamnetin could be identified by TLC. Quercetin showed a good linear relationship at a range of 0.412-1.648 microg, r = 0.999 9, the average recovery was 96.8%, and RSD was 0.9% (n = 6). Kaempferol showed a good linear relationship at a range of 0.021-0.083 microg, r = 0.999 8, the average recovery was 96.9%, and RSD was 2.0% (n = 6). Isorhamnetin showed a good linear relationship at a range of 0.183-0.732 microg, r = 0.999 9, the average recovery was 97.1%, and RSD was 1.6% (n = 6).
CONCLUSIONThe method is accurate with the good reproducibility and can be used for the quality control of Xindi soft capsule.
Capsules ; Chromatography, Thin Layer ; Drugs, Chinese Herbal ; administration & dosage ; chemistry ; isolation & purification ; standards ; Flavonols ; analysis ; Hippophae ; chemistry ; Kaempferols ; analysis ; Plants, Medicinal ; chemistry ; Quality Control ; Quercetin ; analysis ; Reproducibility of Results