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OBJECTIVE: To establish a micellar electrokinetic chromatography(MEKC) method for simultaneous determination of salidroside, tyrosol, ligustroflavone, specnuezhenide, oleanolic acid, and ursolic acid in Ligustri Lucidi Fructus. METHODS: 60 mmol·L-1 borax-10 mmol·L-1 SDS-30 mmol·L-1 hydroxypropyl-beta-cyclodextrin-10% methyl alcohol was used as the buffer solution (pH 9.03). Uncoated fused silica capillary (75 μm×64.5 cm, 56 cm of effective length) was used with separation voltage of 20 kV. The detection wavelength was set at 210 nm. The column temperature was maintained at 25°C, and the sample was injected at 5 kPa×6 s. RESULTS: The calibration curves of the six index components showed good linearity (r>0.95) in the range of the tested concentrations, and the average recoveries of the method were between 94.57% and 102.07% (RSD<5%). CONCLUSION: The method is simple, accurate and reproducible, and can be used for the quality control of Ligustri Lucidi Fructus.
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Objective: Determining the content of five flavonoids in Artemisia frigida by high performance capillary electrophoresis (HPCE) method to provide reference data for the evaluation of processing products of A. frigida. Methods: Treated by different processing technologies, the content of five flavonoids compounds can be determined and compared by HPCE. Results: Regression equations were 5,7,3′-triterhydroxy-4′-methoxyflavone Y = 0.114 3 X + 0.032 7, r = 0.999 8; 5,3′-dihydroxy-6,7,4′-tritermethoxyflavone Y = 0.100 9 X + 0.048 5, r = 0.999 6; quercetin Y = 0.055 5 X + 0.026 8, r = 0.999 6; 5,7,3′-triterhydroxy-6,4′-dimethoxyflavone Y= 0.113 2X-0.016 1, r = 0.999 3; luteolin Y = 0.097 9X-0.029 5, r = 0.999 4. Five kinds of flavonoids were good linear relationship at 1.00-40.00, 10.00-200.00, 5.00-100.00, 1.00-40.00, 1.00-40.00 μg/mL. The average recoveries were 98.44%, 97.75%, 97.73%, 97.98%, and 98.07%. And RSD were 1.60%, 1.03%, 1.57%, 0.94%, and 1.20%. Conclusion: The results reveal that the different processing technologies have different effects on the content determination of five flavonoids compounds in A. frigida. Using the five flavonoids as testing indexes, the best processing technology of A. frigida is heating and drying to constant weight at 60 °C.
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Objective: To establish a micellar electrokinetic chromatography method with high perfor mance capillary electrophoresis (HPCE) fingerprint of Corni Fructus pieces. Methods: Separation was performed on a fused-silica capillary column (64. 5 cm x 75 μm, effective length 56 cm) with 50 mmol/L borax solution -40 mmol/L SDS- 5% acetonitrile (pH 9. 5) as HPCE buffer. The running voltage was 10 kV, the detection wavelength was 240 nm, and column temperature was 18°C. Taking loganin as reference, the data were analysed by Fuzzy Cluster and Fingerprint Similarity Evaluation Software to compare the similarity of samples. Results: HPCE Fingerprint was established with nine common peaks. Conclusion The method is accurate, simple, and suitable to the quality control of Corni Fructus.
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Objective To establish a rapid assay for the determination of methotrexate (MTX) in serum.Method The assay was based on the ultraviolet absorbance of methotrexate at 306 nm. The separation of the drug was done by high performance capillary electrophoresis (HPCE). The bare fused-silica capillary was 60 cm in total length, 50.5 cm in efficient length and 75?m in diameter. The voltage of 25 kV was applied. The running buffer was 75 mmol/L phosphate, pH7.4. The performance of methodology was evaluated.Result The complete separation of MTX was achieved within 10 min. The linearity of the assay was from 1.1 ?mol/L to 1100.0 ?mol/L. The minimal detection limit was 0.55 ?mol/L.The recovery of MTX was from 88.2% to 98.2%. Within-run precision was 4.2% and between-run precision was ~5.4%. Conclusion The result indicated that the method was an effective method for clinical and scientific research with advantages of rapidity, simplicity and accuracy.
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Objective To establish an HPCE method for the determination of oxymatrine in Compound Kushen Colon-specific Capsula.Methods Amphetamine sulfate was used as the internal standard.The separation was obtained with silica capillary column(50 cm ? 50 ?m,effective length 45 cm),30 mmol/L phosphate buffer(pH 5.8)at a constant voltage of 20 kV,and temperature at(25?1)℃,the detective wavelength 214 nm.Results The linear determination range was 30—240 ?g/mL and the average recovery and RSD were 99.54% and 1.85%,respectively.Conclusion The method is simple and accurate,and can be used for quality control of Compoud Kusheng Colon-specific Capsula.
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Object To study the HPCE fingerprinting of Gegen Qinlian Decoction (GQD). Methods A buffer was composed of 30 mmol/L sodium phosphate and 40 mmol/L borate solution. Capillary electrophoresis was performed using a 65 cm (43 cm to detector) ?50 ?m fused-silica capillary tube. Separation voltage was 22 kV, sampling time was 1 s, detected wavelength was 254 nm, and the temperature was maintained at 30 ℃. Results The 27 components in GQD were successfully separated. The observation of methodology was in keeping with quantitatine determination and qualitative study. Conclusion This method can be used for the quality control of the preparation of GQD with good precision.
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Object To develop a high-performance capillary electrophoresis method to determine ferulic acid concentrations in serum of rats treated with Buyang Huanwu Decoction (BHD). Methods Capillary zone electrophoresis was applied for ferulic acid assay, quantitative determination was based on internal standard and detection was carried on by direct UV. The electrolyte buffer was composed of 25 mmol/L borax-methanol (85∶15). Capillary electrophoresis was performed using a 52 cm (30 cm to detector)?50 ?m fused-silica capillary tube. Separation voltage was 20 kV, sampling time was 3 s, detection wavelength was 320 nm, and the temperature was 30 ℃. Results Ferulic acid was successfully separated within 6 min, the recoveries were 97.2% in serum and 103.28% in BHD, respectively. RSD were 3.73% and 0.91% (n=3), respectively. Conclusion This method can supply reference for the determination of ferulic acid in serum samples and BHD.
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Objective To develop a method of quality control for fingerprints of Xinshu Oral Liquid. Methods Based on electrophoregram of ten batches of genuine Radix Angelicae Sinensis (RAS), ten batches of genuine Rhizoma Chuanxiong (RC), and ten batches of genuine Flos Carthami (FC) by high performance capillary electrophoresis (HPCE) to compare the fingerprints between Xinshu Oral Liquid and the genuine medicinal herbs, single herb decoction, nagetive control herb solution, respectively. The fingerprint assignment was made by comparing the UV spectra and relative migration time. Results To compare the fingerprints of ten samples from different batches and single herb, the correlation of peaks between fingerprings was found. Finally the standard fingerprints and the method of quality control were established. Conclusion Based on the fingerprints of ten batches of prearations, an average electro-phoregram was used as the standard fingerprint. There are 27 “common peaks” in the fingerprint, among them 14 from RAS, ten from RC (in which seven are commnon) and nine from FC.
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Objective: The method for separation by capillary zone electrophoresis (CZE) and electrochemical determination of organic acids in fruit juices was developed. Method: In this system, 0.2mmol/L cetylpyridinium bromide (CPB) was used as an electro osmotic flow (EOF) modifier to reverse the direction of EOF. cyclodexfrin ( -CD) was added into running buffer to improve the separation efficiency. Then, the optimal separation conditions were achieved and successfully employed to separate six organic acids, including oxalic, malic, tartaric, succinic, fumaric acid and citric acids. One nano palladium modified carbon paste electrode was used for determination. Results: The calibration curves for all organic acids studied were linear with 2-3 orders (1 10–6-1.0 10–3 mol/L) of magnitude and all the detection limits (S/N=3) were below 2 mol/L. The RSD was between 1.05%-2.15% , and recovery was 93.4% . Conclusion: CZE separation combined with electrochemical detection is suitable for simultaneous determination of organic acids in fruit juices quickly with high sensitivity and selectivity.