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OBJECTIVE： To establish the quality standard for Kazakhstan medicine Peganum harmala. METHODS： Ten batches of P. harmala collected in Xinjiang Kazakh region were selected as research objects to investigate their characteristics. Qualitative identification of harmaline and harmine was conducted by TLC. The contents of water， total ash， acid-insoluble ash and ethanol extract were tested according to Chinese Pharmacopoeia（2015 edition）. The contents of harmaline and harmine were determined by HPLC. The determination was performed on X-bridge C18 column（250 mm×4.6 mm，5 μm） with mobile phase consisted of acetonitrile-ammonium acetate buffer （adjusted to 6 with glacial acetic acid， gradient elution） at the flow rate of 1 mL/min. The detection wavelength was set at 267 nm， and column temperature was 25 ℃. The sample size was 5 μL. RESULTS： TLC identification results showed that 10 batches of medicinal material showed clear spots at the same position as harmaline and harmine reference substances. Water， total ash， acid-insoluble ash should not be more than 12％，22％，2％， respectively； ethanol extract must not be less than 16％. HPLC results showed that the linear ranges of harmaline and harmine were 15.22-301.40，15.09-301.80 μg/mL； RSDs of precision， reproducibility and stability tests were all lower than 4％； average recoveries were 100.22％ and 100.94％（all RSD＜2％）. The determination results showed that the content of total alkaloids （harmaline and harmine） should not be less than 6.5 mg/g. CONCLUSIONS： Based on the original standard， test items are added in this study. TLC method is established to identify harmaline and harmine. HPLC method is established to determine their contents. Established quality standard can be used for comprehensive quality control of P. harmala from Xinjiang Kazakh region.
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Objective: To develop an HPLC-DAD method for the simultaneous determination of five active constituents (chlorogen-ic acid, baicalin, rutin, linarin and apigenin) in Cirsii Herba dispensing granules. Methods: The chromatographic separation was per-formed on a Thermo Hypersil BDS C18column (250 mm×4. 6 mm,5 μm) with gradient elution by 0. 1% phosphoric acid-acetonitrile as the mobile phase at the flow rate of 1. 0 ml·min-1. The detection wavelength was set at 326 nm,and the column temperature was maintained at 35 ℃. Results: Chlorogenic acid, baicalin, rutin, linarin and apigenin were linear within the range of 0. 072-1. 446 μg (r=0.999 7), 0.043-0.864 μg(r =0.999 5), 0.094 2-1.884 μg (r =0.999 7), 0.150-3.000 μg (r =0.999 8) and 0.043-0. 856 μg (r=0. 999 6), respectively. The recovery was 97. 67% , 98. 19% , 97. 92% ,98. 12% and 98. 02% , and the RSDs was 0. 82% , 0. 92% , 1. 25% , 0. 98% and 1. 17% , respectively. Conclusion: The method is accurate, convenient and reproducible in the quality control of multicomponents in Cirsii Herba dispensing granules.
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Objective:To establish a method for the content determination of two ingredients in ktoconazole and clobetasol propio -nate cream.Methods:HPLC was performed on a Kromasil C 18 column (250 mm ×4.6 mm, 5 μm) with the mobile phase of metha-nol-sodium acetate with gradient elution at a flow rate of 1.0 ml· min-1 .The detection wavelength was 239 nm, the column tempera-ture was 30℃and the injection volume was 10 μl.Results:The linear range was 160.30-1282.40 μg· ml-1 for ketoconazole (r=1.0000) and 4.03-32.24μg· ml-1 for clobetasol propionate (r=1.0000).The average recoveries were 100.9％(RSD=0.52％, n=9) and 100.2％(RSD=0.56％,n=9), respectively.Conclusion:The method is accurate with good specificity and high sensi-tivity, which can be used for the detection of ketoconazole and clobetasol propionate .
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Objective:To develop an HPLC method for the simultaneous determination of four phenolic compounds ( monocaffey-ltartaric acid, chlorogenic acid, caffeic acid and chicoric acid) in Herba Taraxaci. Methods:The separation was performed on a Ther-mo C18 column (250 mm × 4. 6 mm, 5 μm) with methanol-0. 2％ phosphonic acid as the mobile phase with gradient elution. The de-tection wavelength was 328 nm, the flow rate was 1. 0 ml·min-1 and the column temperature was 35℃. Results:The linear range of monocaffeyltartaric acid, chlorogenic acid, caffeic acid and chicoric acid was 11.59-115.90 (r = 0.9999), 2.50-24.96(r =0. 9998),2. 27-22. 70(r=0. 9995) and 12. 44-124. 40(r=0. 9998) μg ·ml-1, respectively. The average recovery was 102. 50％(RSD=2. 30％), 99. 29％(RSD=0. 43％), 96. 71％(RSD=0. 78％) and 95. 36％ (RSD=1. 30％), respectively. Conclusion:The method is simple and accurate with good repeatability, which can be used for the quality control of Herba Taraxaci.
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OBJECTIVE:To improve the method for the determination of 2 main components in Ticarcillin disodium and potas-sium clavulanate for injection. METHODS:HPLC was performed on the column of Waters XBridgeTM C18 with mobile phase of 0.01 mol/L ammonium dibasic phosphate solution(pH 7.0)-menthol(80:20,V/V)at a flow rate of 1.0 mL/min,the detection wave-length was 220 nm, column temperature was 30 ℃, and injection volume was 20 μL. RESULTS:The linear range was 1.95-195.22 μg/mL for ticarcillin (r=0.9999) and 0.12-12.18 μg/mL for clavulanate(r=0.9999);RSDs of precision,stability (under 4 ℃) and reproducibility tests were lower than 1.0%;recoveries were 99.3%-100.5%(RSD=0.4%,n=9) and 99.2%-101.0%(RSD=0.7%,n=9). CONCLUSIONS:The method is rapid,accurate and reliable,and can be used for the determination of 2 main components in Ticarcillin disodium and potassium clavulanate for injection.
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Objective:To determinate the substances with high molecular weight in porcine anterior pituitary and adrenal cortex extracts injection. Methods:The HPLC analysis was performed on a TSK-GEL G2000SWXL(7. 8 mm × 300 mm,5 μm) column with the mobile phase of trifluoroacetic acid-acetonitrile-water(0. 05:35:65). The flow rate was 0. 5 ml·min-1, and the detection wave-length was 214 nm. Results:The substances with high molecular weight in porcine anterior pituitary and adrenal cortex extracts injec-tion was below 1%. Conclusion:The method is simple and repeatable, which can be used for the control of the substances with high molecular weight in porcine anterior pituitary and adrenal cortex extracts injection.
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Objective:To establish a GC method for determining the content of amantadine hydrochloride in pediatric paracetamol and amanatadine hydrochloride granules. Methods:The ingredients were separated on an Agilent DB-5 quartz capillary column (30 m ×0.25 mm, 0.25 μm), the carrier gas was N2,and the flow rate was 1 ml·min-1. The column temperature was maintained at 130℃, the injection temperature was 250℃,the detection temperature was 280℃ with an FID as the detector , the injection volume was 2 μl, and the split ratio was 20∶1. Results:A good linear relationship was obtained between the peak area and the concentration of amantadine hydrochloride within the range from 0.103 2 to 6.456 0 mg·ml-1(r =0.999 9). The average recovery was 100.18%(RSD=0. 11%, n=6). Conclusion:The method is specific, accurate, reliable and reproducible, which can be used in the quality control of pediatric paracetamol and amanatadine hydrochloride granules.