2.Capillary electrophoresis method for the determination of flavonoids.
Ming-Lei CHEN ; Wei HU ; Chao ZHANG ; Yun FANG
Acta Pharmaceutica Sinica 2011;46(8):883-889
Due to their biological and physiological importance, flavonoids received considerable attention in the literature. This review discusses the widely used analytical method i.e. capillary electrophoresis (CE) including the chiral flavonoids separation and the hyphenation of CE and MS. Techniques used for enhancement of sensitivity such as stacking, sweeping, isotachophoresis etc. were also discussed.
Capillary Electrochromatography
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methods
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Electrophoresis, Capillary
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methods
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Flavonoids
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analysis
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isolation & purification
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Isotachophoresis
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methods
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Mass Spectrometry
;
methods
3.Determination of cytidine and adenosine in cordyceps by monolithiccapillary electrochromatography.
Huaizhong GUO ; Kaishun BI ; Yuqing SUN
China Journal of Chinese Materia Medica 2009;34(5):587-590
OBJECTIVETo develop a capillary electrochromatography method for determination of cytidine and adenosine in cordyceps with monolithic column.
METHODThe total length of the home-made ploy-butyl methacrylate (PBMA) monolithic capillary electrochromatographic column was 34.5 cm with the effective length of 26.0 cm. The mobile phase was 20 mmol x L(-1) borax solution (adjusted pH to 3.5 using acetic acid); the operation voltage was 15 kV; sample injection pressure was 6 bar x 0.1 min; column temperature was 30 degrees C and the detection wavelength was set at 214 nm. The internal standard solution was 100 mg x L(-1) trimethoprim solution [ethanol-mobile phase (1 : 1) was used as the solvent].
RESULTThe results indicated that the concentrations of cytidine and adenosine within the range of 12.5-125 mg x L(-1) were linearly correlated with the relative peak areas, and the correlative coefficients (r) were 0.999 8 and 0.999 3, respectively. The LOD (S/N = 3) and LOQ (S/N = 10) of cytidine were 2.14 and 7.14 mg x L(-1), and those of adenosine were 1.88 and 6.25 mg x L(-1). The average recoveries of the two nucleosides were from 97.2% to 103.5% with relative standard deviation (RSD) within 0.9%-2.6% in three levels.
CONCLUSIONThe method is effective and credible. It can be used to determine the contents of cytidine and adenosine in cordyceps.
Adenosine ; analysis ; Capillary Electrochromatography ; methods ; Cordyceps ; chemistry ; Cytidine ; analysis ; Sensitivity and Specificity
4.Regulations of residual solvents in pharmaceuticals and advances in the research of its analytical methods.
Acta Pharmaceutica Sinica 2007;42(12):1237-1242
If the presence of residual solvents in pharmaceuticals exceeds tolerance limits as suggested by safety data, they may be harmful to the human body or the environment. It is because of this that the determination of residual solvents receives a great deal of attention. This paper reviews in detail the changes in the regulations on residual solvents in pharmaceuticals in leading pharmacopoeias, and the advances in the techniques involved, especially, the recent advances in the analytical techniques are summarized. At the end, the authors introduce the prospect of the expert system for determining residual solvents in pharmaceuticals based on the studies of their research group.
Capillary Electrochromatography
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Chromatography, Gas
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Drug Contamination
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prevention & control
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Drug and Narcotic Control
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Pharmaceutical Preparations
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chemistry
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Quality Control
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Solvents
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analysis
6.Determination of tetrandrine and fangchinoline in Radix Stephaniae tetrandrae and its preparation by nonaqueous capillary chromatography.
Yu-Qin LI ; Xing-Guo CHEN ; Yong-Xiu QI ; Ke LI ; Bao-Xiu JIA ; Cai-Hong LIU ; Ming-Liang CAO
China Journal of Chinese Materia Medica 2007;32(19):1992-1995
OBJECTIVETo establish a new method for the determination of fangchinoline and tetrandrine in Stephania tetrandra and Fengtongan capsule by noanqueous capillary electrophoresis.
METHODSeparation was carried out in an uncoated fused capillary (50 cm x 75 microm i.d.) with a running buffer containing 50 mmol x L(-1) ammonium acetate, 1.0% acetic acid and 20% acetonitrile in methanol. A separation voltage of 20 kV and a UV detector wavelength at 214 nm were adopted. Sample was introduced from the anode.
RESULTThe calibration ranges were 1.00, 500 mg x L(-1) for both analytes. Under the optimum conditions, the relative standard deviation (RSD, n = 6) for the migration time of each analyte were 0.09%, 1.9% (intra-day) and 0.63%, 1.9% (inter-day); The RSD for the peak area of each analyte were 0.45%, 5.9% (intra-day) and 2.3%, 5.6% (inter-day), respectively. The contents of the analytes were determined easily with average recoveries 102% for fangchinoline and 105% for tetrandrine in S. tetrandra and 94.6% for fangchinoline and 98.7% for tetrandrine in Fengtongan capsules, respectively.
CONCLUSIONThe proposed method is simple, rapid, accurate and higher repeatable, and can be used to control of the quality of S. tetrandra and Fengtongan capsules.
Benzylisoquinolines ; analysis ; Calibration ; Capillary Electrochromatography ; methods ; Capsules ; Drugs, Chinese Herbal ; chemistry ; isolation & purification ; standards ; Plant Roots ; chemistry ; Plants, Medicinal ; chemistry ; Quality Control ; Reproducibility of Results ; Stephania tetrandra ; chemistry
7.Safety destruction of tetramethylene disulfotetramine and its medical waste.
Xiao-hua LI ; Zhong-hui CHEN ; Yan-fei LU ; Xiao-wei GE ; Jun GUO
Chinese Journal of Preventive Medicine 2005;39(2):88-90
OBJECTIVETo develop suitable methods for safety destruction of tetramethylene disulfotetramine (TETS) and the medical wastes polluted by TETS.
METHODSThe chemical stability of TETS was evaluated under the conditions of acid, alkali and high temperature. TETS was treated with sodium hydroxide, hydrochloric acid, sulfuric acid and nitric acid under various treatment conditions, i.e. concentration, temperature and time, followed by determining remaining TETS using gas chromatograms to estimating the degradation efficiency of TETS. TETS was put into ampoule and heated under the different conditions of temperature and time. After heat treatment, TETS residue was determined. For evaluating the absorption factor of active carbon to TETS in water and blood, active carbon was added into the water and blood with content of TETS, incubated at room temperature for 24 hours, and then determined the remaining TETS in water and blood.
RESULTSThe complete degradation of TETS was achieved by one of the following treatments: heating with 6.0 mol/L hydrochloric acid at 100 degrees C for half an hour, heating with 3.0 mol/L hydrochloric acid or 6.0 mol/L sodium hydroxide at 100 degrees C for 3 hours, mixing with concentrated sulfuric acid or nitric acid at room temperature for 24 hours, and dry heating at 300 degrees C for 4.5 hours. Active carbon showed a marked effectiveness in absorbing the TETS in blood and water, with the mean absorption efficiency of over 90%.
CONCLUSIONSThe results of this study suggest that TETS powder should be degraded by acid or alkali, and that the solid medical wastes polluted by TETS should be destroyed at high temperature. For the blood and water having contents of TETS, the active carbon should be used as to absorbing the TETS and then be destroyed at high temperature.
Bridged-Ring Compounds ; chemistry ; Capillary Electrochromatography ; Chromatography, Gas ; Hydrochloric Acid ; chemistry ; Medical Waste Disposal ; methods ; Nitric Acid ; chemistry ; Sodium Hydroxide ; chemistry ; Sulfuric Acids ; chemistry ; Temperature