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OBJECTIVE： To establish a method for quality control of Peony pollen buccal tablets， and to provide reference for the formulation of quality standard. METHODS： TLC method was used for qualitative identification of paeoniflorin， kaempferol and luteolin in Peony pollen buccal tablets according to 2015 edition of Chinese Pharmacopeia （part Ⅳ）. The contents of paeoniflorin and oxypaeoniflorin in Peony pollen buccal tablets were determined by dual-wavelength HPLC method [The determination was perform on Agilent TC-C18 column with mobile phase consisted of acetonitrile （A）-0.1％ phosphoric acid solution （B） with gradient elution at the flow rate of 1.0 mL/min. The detection wavelength was set at 230 nm for paeoniflorin and 258 nm for oxypaeoniflorin. Sample size was 20 μL]. RESULTS： TLC identification of paeoniflorin， kaempferol and luteolin showed that the same color characteristic spots of control chromatogram appeared in the corresponding positions of sample chromatogram without interference from negative samples. The linear range of paeoniflorin and oxypaeoniflorin were 7.2-86.4 μg/mL and 2.72-32.64 μg/mL（r≥0.999 7），respectively. The average recoveries were 99.12％ and 98.65％， and RSD were 1.54％ and 2.53％（n＝6），respectively. RSDs of precision （n＝6）， stability （n＝8） and reproducibility （n＝6） tests were all lower than 3.0％. CONCLUSIONS： The method is simple and reproducible， and can be used for quality control of Peony pollen buccal tablets.
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Objective: To establish an HPLC determination method for the quantitative indicators in Qubai granules( stilbene gly-cosides, ferulic acid and paeonol). Methods: A dual-wavelength HPLC assay was used with the following conditions: a chromatogra-phy column ODS (150 mm×4. 6 mm, 5 μm) was used, the mobile phase was methanol: 0. 1% phosphoric acid with gradient elution, the column temperature was 35℃, and the injection volume was 10 μl. Results: The linear ranges of the three active constituents were 1.56-156.00 μg·ml-1(r stilbeneglycoside=0.999 8)、1.00~100.00 μg·ml-1(rferulicacid=0.999 8),1.61~161.00 μg·ml-1(rpaeonol=0. 999 7), respectively, and the average recoveries of the three constituents were between 100. 33% and 100. 76% with the RSDS less than 2% (n=6). Conclusion: The method is simple, stable and reliable, which can be used for the quality control of Qubai granules.
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OBJECTIVE:To establish a method for simultaneous determination of (R,S)-goitrin and chlorogenic acid in Banchai oral liquid.METHODS:The dual-wavelength HPLC method was adopted.The determination was performed on Wondasil C18 column with mobile phase consisted of acetonitrile-0.1％ phosphoric acid (11∶89,V/V) at the flow rate of 1.0 mL/min.The detection wavelengths were 245 nm for (R,S)-goitrin and 327 nm for chlomgenic acid.The column temperature was 30 ℃,and injection volume was 10 μL.RESULTS:The linear ranges were 4.05-40.51 μg/mL for (R,S)-goitrin (r=0.999 9),29.41-294.05 μg/mL for chlorogenic acid (r=0.999 9).The limits of quantification were 3.32,2.45 ng,limits of detection were 1.00,0.74 ng.RSDs of precision,stability and reproducibility tests were lower than 1.0％;the recoveries were 98.46％-101.06％ (RSD=0.98％,n=9) and 98.18％-100.78％ (RSD=0.86％,n=9).CONCLUSIONS:The method is simple,accurate,sensitive and reproducible,and can be used for simultaneous determination of (R,S)-goitrin and chlorogenic acid in Banchai oral liquid.
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OBJECTIVE:To establish a method for simultaneous determination of (R,S)-goitrin and chlorogenic acid in Banchai oral liquid.METHODS:The dual-wavelength HPLC method was adopted.The determination was performed on Wondasil C18 column with mobile phase consisted of acetonitrile-0.1％ phosphoric acid (11∶89,V/V) at the flow rate of 1.0 mL/min.The detection wavelengths were 245 nm for (R,S)-goitrin and 327 nm for chlomgenic acid.The column temperature was 30 ℃,and injection volume was 10 μL.RESULTS:The linear ranges were 4.05-40.51 μg/mL for (R,S)-goitrin (r=0.999 9),29.41-294.05 μg/mL for chlorogenic acid (r=0.999 9).The limits of quantification were 3.32,2.45 ng,limits of detection were 1.00,0.74 ng.RSDs of precision,stability and reproducibility tests were lower than 1.0％;the recoveries were 98.46％-101.06％ (RSD=0.98％,n=9) and 98.18％-100.78％ (RSD=0.86％,n=9).CONCLUSIONS:The method is simple,accurate,sensitive and reproducible,and can be used for simultaneous determination of (R,S)-goitrin and chlorogenic acid in Banchai oral liquid.
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Objective To establish an HPLC method for simultaneous determination of loganin, chiratin, secoxyloganin, rosmarinic acid and calceolarioside B in Shuangxiangpaishi granules. Method HPLC colunmn was Alltima C18 column (4.6 mm×250 mm, 5 μm); mobile phase consisted of acetonitrile-methanol (1: 3) (A) -0.1% phosphate acid solution (B) with gradient elution; the column temperature was 35°C; the flow rate was 1.0 ml/min; all the injection volume was 20 μl; loganin, chiratin and secoxyloganin were detected at 240 nm, rosmarinic acid and calceolarioside B were detected at 330nm. Results The above mentioned five main ingredients had linearity in the given concentration range at 5.91-118.20 μg/ml (r=0.9995), 4.10-82.00 μg/ml (r=0.9991), 8.13-162.60 μg/ml (r=0.9993), 12.57-251.40 μg/ml (r=0.9998), 4.95-99.00μg/ml (r=0.9997), respectively. The average recoveries (n=6) and RSD were 96.88 (1.31), 99.09 (1.47%), 98.29 (1.59), 98.82 (1.42) and 97.51 (0.86), respectively. Conclusion This dual-wavelength HPLC method could simultaneously determine the contents of the five ingredients in Shuangxiangpaishi granules and can be used to evaluate their quality. The method is simple, accurate, sensitive and repeatable. It could be used as an efficient strategy for systematic quality evaluation of Shuangxiangpaishi granules.
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OBJECTIVE:To establish a method for the contents determination of tanshinol,protocatechuic aldehyde,ferulic ac-id and salvianolic acid B in Yixinshu capsule. METHODS:Dual-wavelength HPLC was performed on the column of Eclipse XDB-C18 with mobile phase of 0.5%phosphoric acid-methanol-acetonitrile(gradient elution)at the flow rate of 1.0 ml/min,the de-tection wavelength was 280 nm(tanshinol,protocatechuic aldehyde,salvianolic acid B)and 320 nm(ferulic acid),column tempera-ture was 30℃and volume was 10 μl. RESULTS:The linear range of tanshinol,protocatechuic aldehyde,ferulic acid and salvianolic acid B were respectively 9-144μg/ml(r=0.999 9),0.5-8μg/ml(r=0.999 9),0.65-10.4μg/ml(r=0.999 9)and 221.25-3 540μg/ml (r=0.999 9);RSDs of precision,stability and reproducibility tests were no more than 1.90%;the average recovery was respective-ly 100.8%(RSD=1.65%,n=9),100.1%(RSD=2.87%,n=9),100.1%(RSD=3.01%,n=9) and 99.4%(RSD=2.05%,n=9). CONCLUSIONS:The method is simple and reproducible,and can be used for the quality control of Yixinshu capsule.
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OBJECTIVE:To establish a method for simultaneous determination of the contents of ligustroflavone,specnuezhe-nide,demethylwedelolactone and wedelolactone in Zibu ganshen pill. METHODS:Dual-wavelength HPLC was performed on the column of Elite C18 with mobile phase of acetonitrile-0.5%acetic acid(gradient elution)at flow rate of 0.9 ml/min,column temper-ature was 25 ℃,detection wavelengths were 224 nm(0-30 min) and 351 nm (30-50 min),and the injection volume was 20 μl. RESULTS:The linear range was 6.75-135.00μg/ml(r=0.999 5)for ligustroflavone,6.54-130.80μg/ml(r=0.999 8)for specnuezhe-nide,4.90-98.00μg/ml(r=0.999 4)for demethylwedelolactone and 6.42-128.40μg/ml(r=0.999 6)for wedelolactone;RSDs of pre-cision,stability and reproducibility tests were no more than 1.25%;average recoveries were 96.15%-99.96%(RSD<2%,n=6). CONCLUSIONS:The method is rapid,sensitive and accurate,and can be used for the contents determination of ligustroflavone, specnuezhenide,demethylwedelolactone and wedelolactone in Zibu ganshen pill.
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Objective To determine ferulic acid and paeoniflorin in Ankong Zhongzi Wan by HPLC under dual wavelength ultraviolet detection. Methods Ferulic acid and paeoniflorin were separated by Waters SymmetryShield-C18 column (4.6 mm × 250 mm, 5 μm) with gradient elution of acetonitrile-0.1%phosphoric acid as the mobile phase at a flow rate of 1.0 mL/min. The detection wavelength was 230 nm and 323 nm. Results The linear relationship of ferulic acid and paeoniflorin was good in the range of 0.058 2-0.582 4 μg (r=0.999 4) and 1.664-16.64 μg (r=0.999 6), and the average recovery rate was 97.77% (RSD=1.88%) and 98.84% (RSD=1.96%), respectively. Conclusion The method is accurate and quick for determining the two effective components in Ankong Zhongzi Wan, and can be used for its quality control.