ABSTRACT
Objective To establish a method for the simultaneous determination of Forsythoside A, Phillyrin, (R,S)-Epigoitrin, Chlorgenic Acid and Isochlorogenic Acid A by HPLC, and test 16 batches of samples from 14 manufacturers. Methods The test was performed on Kinetex EVO C18 column (150 mm × 4.6 mm, 5 μm) with the column temperature at 35 ℃ . The gradient elution was adopted with the mobile phase of acetonitrile and 0.3% phosphoric acid aqucous at a flow rate of 1.0 ml/min. The detection wavelength of (R,S)-Epigoitrin and Phillyrin were set as 236 nm, the detection wavelength of Forsythoside A, Cholorogenic Acid and Isochlorogenic Acid A were set as 327 nm. Results The good linear relationships were displayed within the linear range of 0.050 45-2.018 00 μg for Forsythoside A (r=0.999 9), 0.018 21-0.728 40 μg for Phillyrin (r=0.999 9), 0.010 16-0.406 40 μg for (R,S)-Epigoitrin (r=0.999 9), 0.006 60-0.263 90 μg for Cholorogenic Acid (r=0.999 9) and 0.0040 44~0.161 76 μg for Isochlorogenic Acid A ( r=0.999 5). The RSDs of reproducibility and stability tests were lower than 2%; recoveries were 97.01%, 98.28%, 99.35% and 96.21%, RSD were 3.19%, 1.19%, 0.81%, 2.88% and 2.96%. The content ranges of Forsythoside A, Phillyrin, (R,S)-Epigoitrin, Chlorgenic Acid and Isochlorogenic Acid A from 16 batches of samples from 14 manufacturers were 0.057 43-1.508 71 mg/g, 0.017 72-0.350 15 mg/g, 0.005 68-0.177 13 mg/g, 0.007 53-0.226 33 mg/g and 0.00308-0.11908 mg/g. Conclusions The established method is simple and accurate, and has a good repeatability. It can be used for the quality analysis of Forsythoside A, Phillyrin, (R,S)-Epigoitrin, Chlorgenic Acid and Isochlorogenic Acid A. The content of the tested chemical components from 16 batches of samples from 14 manufacturers have significant differences which indicate that a reinforcement of the quality control is needed.
ABSTRACT
Objective: To establish the HPLC chemical fingerprints of Wuwei Xiaoduyin Oral Liquid (WXOL) and simultaneous determination method for six major characteristic components in this herbal preparation, i.e. chlorgenic acid, luteoloside, luteolin, linarin, caffeic acid, and esculetin. Methods: Both chemical fingerprint analysis and quantitative determination were implemented by Agilent 1260 high performance liquid chromatography system with an Agilent 5 TC-C18 column (250 mm × 4.6 mm, 5 μm). A gradient elution program, with the mobile phase of 0.5% glacial acetic acid aqueous solution (A) and methanol (B), was employed as following: 0—10 min, 10%—32% B; 10—20 min, 32% B; 20—25 min, 32%—46% B; 25—31 min, 46%—48% B; 31—41 min, 48%—80% B at the flow rate of 1.0 mL/min. The detection wavelength and column temperature were set at 320 nm and 30 ℃, respectively. Additionally, fingerprint similarity of 10 batches of WXOL was evaluated by software “Similarity Evaluation System for Chromatographic Fingerprint of TCM” published by GPC (Version 2012). The amounts of six characteristic components in WXOL were also simultaneously determined. Results: The common fingerprint pattern derived from 10 batches of samples was obtained with the similarity over 0.98 and 17 common peaks defined. Meanwhile, some common peaks were identified via peak pattern match with standard substances, showing that the peak No.5, No.7, No.8, No.12, No.16, and No.17 was chlorgenic acid, esculetin, caffeic acid, luteoloside, linarin, and lutelin, respectively. Chlorgenic acid content range of 54.038 3—105.551 1 μg/mL, esculetin content range of 4.122 1—31.359 9 μg/mL, caffeic acid content range of 2.413 0—4.420 7 μg/mL, luteoloside content range of 4.042 8—11.312 8 μg/mL, linarin content range of 3.866 3—46.271 9 μg/mL, and luteolin content range of 0.990 8—2.126 8 μg/mL. In combination with the non-significant difference of multiple characteristic components content among 10 batches of samples, the quality of home-made WXOL would be stable. Conclusion: A novel quality control method, which is HPLC fingerprint in combination with simultaneous quantitative analysis of multiple components, was established in this study, with high repeatability and reliability. Therefore, this method provides an applicable approach for the quality control of WXOL.
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The content of chlorogenic acid in Xiaoer Jiebiao Oral Liquid was determined by HPLC.ODS column was applied.Mobile phase was methanol_1% acetic acid(25∶75),wavelength of detector was 328nm.Samples were extracted with methanol on ultrasonic vibrator.In this method,the linera range of chlorogenic acid is 0.232 ～ 1.16 ?g,the correlation coefficient is 0.9994 ,and the mean recovery is 98.44%. The results showed that this method is simple,quick and reproduciple.
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Objective To establish a method for the content determination of c hlorogenic acid in Yinren Granules. Methods The content of chlorogenic acid wa s detected by HPLC. HPLC was performed with Shim- Pack CLC- ODS column(150? 6.0 mm, 5 ? m) at room temperature, 3 % methyl alcohol- methanol( 79 ∶ 2 1) as mobile phase, the detection wavelength at 327 nm, the flow rate being 1. 2 mL/min and sample loop volume being 10 ? L. Results Chlorogenic acid has a good linearity within 0.102～ 1.02? g (r=0.999)and the average recovery was 98. 17 % with RSD being 1.31 % . Conclusion This method is simple, accurate and can be used for the quality control of Yinren Granules.
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Objective: To develop a method for determination of chlorgenic acid in Shuangyin Solution.Methods: HPLC with Hypersil-ODS column (4.6?250mm,5?m) was used. The mobile phase was acetonitrile-water-acetic acid glacial (10∶110∶3). The detective wavelength was 328nm.Results: The linear range was from 0.0568 ～0.2840mg/mL. The average recovery was 100.16%.Conclusion: The method is simple, rapid and accurate. It can be used to determine chlorgenic acid in Shuangyin Solution.
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OBJECTIVE:To establish the quality criteria for Qingshujiedu granules.METHODS:Thin-layer chromatography(TLC) was employed to make qualitative determination of herba menthae,radix glycyrrhizae,and spica prunellae.While high performance liquid chromatography(HPLC) was applied for the determination of chlorogenic acid in flos lonicerae in Qingshujiedu granules.RESULTS:The chromatograms of herba menthae,radix glycyrrhizae,and spica prunellae obtained through TLC presented the spots of the same colors with those in the corresponding places in the chromatograms of the control articles.The content of chlorogenic acid was linear with the peak area in the range of 0.091?g～0.53?g;The average recovery was 97.16%(RSD=1.15%).CONCLUSION:These methods are accurate and reliable with a strong specificity and can be used for the quality control of Qingshujiedu granules.