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In Korea and China, ilaprazole is a widely used proton pump inhibitor in the treatment of gastric ulcers. In this study, a specific and sensitive LC-MS/MS method has been developed and validated for the quantification of ilaprazole enantiomers in the rat plasma, using R-lansoprazole as the internal standard. The enantioseparation was achieved on a CHIRALPAK AS-RH column (4.6 mm × 150 mm, i.d. 5μm), with a mobile phase composed of 10 mM ammonium acetate aqueous solution and acetonitrile (60:40, V/V), at a flow-rate of 0.5 mL/min. The method was validated over the concentration range of 0.5-300 ng/mL for both, R- and S -ilaprazole. The lower limit of quantification was 0.5 ng/mL for both enantiomers. The relative standard deviation (RSD) of intra- and inter-day precision of R-ilaprazole and S-ilaprazole was less than 10.9％, and the relative error accuracy (RE) ranged from -0.5％-2.0％. Finally, the method was successfully evaluated in rats in a stereoselective pharmacokinetic study of the ilaprazole racemate.
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OBJECTIVE:To establish a RP-HPLC method for the determination of imperatorin in Qingwen jiedu tablets(heat-clearing and detoxifying agent).METHODS:The chromatographic separation was performed on Diamonsil-C18(250 mm?4.6 mm,5 ?m)with column temperature kept at 35 ℃.The mobile phase consisted of methanol-water(70∶30)at a flow rate of 0.8 mL?min-1 with detection wavelength set at 300 nm.RESULTS:The linear range of imperatorin was 2.7～27.0 ?g?mL-1(r=0.999 9)with its average recovery at 98.9%(RSD=1.44%,n=6).CONCLUSION:The established method was proved to be well-separated,sensitive,accurate and applicable for the quality control of Qingwen jiedu tablets.
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OBJECTIVE:To establish capillary electrophoresis method for the determination of imperatorin and isoimperatorin in Yuanhu zhitong tablet. METHODS:The separation was performed on a uncoated fused silica capillary (55 cm?75 ?m ID,effective length of 47 cm) with 20 mmol?L-1 NaH2PO4+100 mmol?L-1 SDS+80%formamide as buffer solution (pH=7.12). The separation voltage was 15 kV and the sample was injected by gravity (5 s,15 cm). The detection wavelength was 254 nm. RESULTS:The linear range of imperatorin and isoimperatorin were 8.0～40.0 ?g?mL-1(r=0.998 7) and 4.0～20.0 ?g?mL-1(r=0.999 0). The average recovery was 101.3% for imperatorin (RSD=3.24%,n=6) and 100.2% for isoimperatorin(RSD=1.44%,n=6). CONCLUSION:The method is convenient,rapid and accurate for the quality control of Yuanhu zhitong tablet.
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OBJECTIVE:To determine the content of shikonin in Arnebia euchroma by HPCE-UV.METHODS:The separation was performed on uncoated fused silica capillary column (53 cm?50 ?m ID,46 cm effective length).2.0 mmol?L-1 H3BO3,6.0 mmol?L-1 triethylamine buffer solution and 5.0 mmol?L-1?-CD was used as background electrolyte,14 kV separation voltage and time of gravity injection 15 s (25 cm).The detection wavelength was set at 516 nm.RESULTS:The linear range of shikonin was 7.2～36.0 ?g?mL-1(r=0.999 0) with an average recovery of 100.15%(RSD=1.68%,n=6).CONCLUSION:The method is convenient,rapid,accurate and reliable for the content determination of shikonin in A.euchroma.
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Objective Using the contents of naphthaquinine and shikonin as the indices,the influences of ultrasonic extraction and soxhlet extraction on the active constituents in Arnebia euchroma(Royle)Johnst.were studied.Methods An orthogonal design was applied.Naphthaquinine content was determined by spectrophotometry and shikonin content by HPLC.The extraction rate of the two extracting methods was compared to optimize the process condition.Results By using the two extracting methods,particle size had an obvious effect on the extraction rate of naphthaquinine(the bigger particle,the higher extraction rate),but had no effect on the extraction rate of shikonin;the solvent of ethanol showed different effects on the extraction rate of active constituents by using the two extraction methods,the extraction rate being higher by ultrasonic extraction while lower by soxhlet extraction.Conclusion Ultrasonic extraction is efficient,and with energy and time saving in extracting active constituents of Arnebia euchroma(Royle)Johnst.,which is superior to soxhlet extraction.
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AIM: To determine the content of(+)-catechin and (-)-epicatechin and berberine hydrochloride in Wangying Capsule(Rhizoma Picrorhizae,Rhizoma Coptidis,Catechu,etc.). METHODS: A RP-HPLC method was established.The chromatographic column was Diamonsil-C_(18).The mobile phase was 0.04 mol/L citric acid-N,N-dimethylformamide-tetrahydrofuran(40∶8∶2) for determining(+)-catechin and(-)-epicatechin with the flow rate of 1.0 mL/min,and the detection wavelength of 280 nm.The mobile phase was acetonitrile-water(52∶48)(including 0.34% potassium dihydrogen phosphate and 0.17% sodium dodecyl sulfate) for determining berberine hydrochloride with the flow rate of 1.0 mL/min,and the detection wavelength of 265 nm. RESULTS: The average recoveries for(+)-catechin and(-)-epicatechin and berberine hydrochloride were 100.9% and 99.9% and 97.0%,precision of the method were 2.52% and 2.53% and 2.70%(RSD,n=6),respectively. CONCLUSION: The method can be used for quantitative determination of the preparation.