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Objective: To establish a fingerprint method of Baimai Ointment (BO) and determine the content of its main components. The BO of 14 batches from two production areas was scientifically and comprehensively evaluated based on multivariate statistical analysis, which provided the basis for the quality control. Methods: HPLC method was used to determine the content of liquiritin, ammonium glycyrrhizinate, nardosinone and curcumin in BO, and the fingerprint of BO was established. The fingerprint similarity analysis, cluster analysis, principal component analysis (PCA) and factor analysis were performed to comprehensively evaluate the different batches of BO in two producing areas. Results: The methodological determination of liquiritin, ammonium glycyrrhizinate, nardosinone and curcumin met the requirements, and the content was 0.051-0.200 mg/g, 0.136-0.622 mg/g, 0.030-0.345 mg/g, 0.001-0.069 mg/g, respectively. The established fingerprints of BO were calibrated with 17 common peaks. Three chromatographic peaks of liquiritin, ammonium glycyrrhizinate and nardosinone were identified by reference. The similarity of 14 batches of sample was greater than 0.975. In the cluster analysis, 14 batches of BO from two producing areas can be divided into four categories, among which batches S1-S11 produced by Linzhi City of Tibet were grouped into one category. And S12 produced in Lanzhou City of Gansu Province was clustered into one class, and S13 was clustered into one class, S14 was grouped into one class. The results of PCA and factor analysis showed that the comprehensive scores of the three batches of S12-S14 produced in Lanzhou City of Gansu Province were higher than the 11 batches of S1-S11 produced by Linzhi City of Tibet, presumably because of the changes in production conditions or sources of medicinal materials. The result was consistent with cluster analysis. Conclusion: This study is the first to establish a scientific and reliable quality control method of Tibetan medicine BO based on multi-component determination, fingerprint and multivariate statistical analysis. It can be used not only for the quality control of Baimai Ointment, but also for the comprehensive evaluation of batch quality consistency. It provides reference for the improvement of the quality standard of BO and the quality evaluation among Chinese medicine batches.
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Objective: To establish an HPLC fingerprint of classical named Linggui Zhugan Decoction and determination method of the content of three compounds, and provide reference for the study of the material basis of the classical Linggui Zhugan Decoction. Methods: The method was performed by high performance liquid chromatography with CNW Athena C18 (250 mm × 4.6 mm, 5 μm) and gradient elution with acetonitrile (A)-0.1% phosphoric acid (B) as the mobile phase, gradient elution: 0-10 min, 5%-10%; 10-20 min, 10%-15% A; 20-50 min, 15%-30% A; 50-75 min, 30%-40% A; 75-95 min, 40%-50% A; 95-111 min, 50%-95% A. The flow rate was 1.0 mL/min, the injection volume was 10 μL, and the column temperature is 30 ℃. The fingerprint and the detection wavelength of glycyrrhizin and ammonium glycyrrhizinate were 230 nm, and cinnamic aldehyde was 290 nm. The chromatographic fingerprint evaluation system published by the State Pharmacopoeia Commission (2012 Edition) was used to establish the fingerprint of 10 batches of Lingguizhugan decoction, and the content of three kinds of index components were determined simultaneously by the established HPLC method. Results: The research on the 10 batches of Lingguizhugan soup showed that the fingerprint similarity was greater than 0.9, and 24 common peaks were calibrated, and the peak resolution was good. The content determination results showed that the content of glycyrrhizin and ammonium glycyrrhizinate was high. According to the methodological investigation, the three components showed a good linear relationship within a certain concentration range; The precision RSD values were all less than 1.0%; The average recovery rates of glycyrrhizin, cinnamaldehyde and ammonium glycyrrhizinate were 98.35%, 101.51%, and 102.59%, respectively. The RSD is less than 2.5%; The sample is stable within 48 h, and the method has good repeatability. Conclusion: The fingerprint method and the determination method of three components in the traditional Chinese medicine classical prescription named Linggui Zhugan Decoction established in this study are simple, stable, accurate and reliable, and can be used for the quality control of the Linggui Zhugan Decoction.
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Objective To study the chemical constituents and effects of crude and processed Pinelliae Rhizoma. Methods The contents of inosine, guanosine, adenosine, succinic acid, ephedrine hydrochloride, liquiritin, glyeyrrhizie acid, and 6-gingerol of Pinelliae Rhizoma, Pinelliae Rhizoma Praeparatum cum Alumine, Pinelliae Rhizoma Praeparatum cum Zingibere et Alumine, and Pinelliae Rhizoma Praeparatum were detected by HPLC. The pharmacodynamics of the traditional efficacy of expectorant and cough relieving was studied by stimulating mice with phenol red and concentrated ammonia in the trachea of mice. Results The contents of inosine, guanosine, adenosine, succinic acid, and ephedrine hydrochloride decreased significantly after processing, and inosine was not detected in Pinelliae Rhizoma Praeparatum cum Alumine. Compared with the three processed products, the content of inosine, guanosine, adenosine and succinic acid was the highest in the Pinelliae Rhizoma Praeparatum cum Alumine, the lowest was in Pinelliae Rhizoma Praeparatum cum Zingibere et Alumine, and in consistent with the effect of resolving phlegm. The four components were the active components of resolving phlegm effect. Adding alumen during Pinelliae Rhizoma Praeparatum cum Alumine processing has also enhanced its effectiveness. Pinelliae Rhizoma Praeparatum has the strongest antitussive effect, followed by Pinelliae Rhizoma, Pinelliae Rhizoma Praeparatum cum Alumine and Pinelliae Rhizoma Praeparatum cum Zingibere et Alumine. Adding licorice and lime water during Pinelliae Rhizoma Praeparatum processing, licorice (peak 6: liquiritin, peak 7: ammonium glycyrrhizinate) had a powerful antitussive effect and enhanced its antitussive effect. After processing by ginger and white peony, ginger (peak 8: 6-gingerol) is good at warming middle energizer to arrest vomiting, thus enhance antiemetic effect and weaken phlegm, cough effect of Pinelliae Rhizoma Praeparatum cum Zingibere et Alumine. Conclusion The chemical composition and efficacy of Pinelliae Rhizoma have changed after being processed, and different processing methods have different effects on its chemical composition and efficacy.
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Objective To establish fingerprint of Jinsangqi Kangdu Dropping Pills by HPLC; To control the quality of the preparation. Methods Waters XSELECT CSH-C18 chromatographic column (4.6 mm × 150 mm, 5 μm) was used and eluted with acetonitrile - 0.1% phosphoric acid solution gradient at the flow rate of 1.0 mL/min. The detection wavelength was 260 nm with column temperature of 30 ℃. Using calycosin-7-O-β-D-glucopyranoside, rutin, liquiritin, hyperoside, quercetin and ammonium glycyrrhizinate as the object references, ten batches of Jinsangqi Kangdu Dropping Pills were tested and analyzed by similarity comparison.Results Fringerprint spectrum of Jinsangqi Kangdu Dropping Pills had 24 common peaks in total, and characteristic spectrums of Hypericum Perforatum, Mori Cortex, Astragali Radix and Glycyrrhizae Radix et Rhizoma had been found, while similarity of HPLC fingerprint was more than 0.9 among those batches of samples. Conclusion Using HPLC fingerprint can evaluate the Jinsangqi Kangdu Dropping Pills quality totality,which can provide references for improving the quality control of the preparation.
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Objective: To analyze 167 batches of Weiling granules according to the quality standard and exploratory research, and evaluate the overall quality and standard condition of the preparation. Methods: A TLC method was established for the identification of Atractylodis macrocephalae Rhizoma;an HPLC method was established for the fingerprint and the content determination of paeoniflorin, tetrahydropalmatine and ammonium glycyrrhizinate. An Agilent Poroshell120,SB-C18analytical column (100 mm×4. 6 mm, 2. 7 μm) was employed with gradient elution of acetonitrile-0. 1% phosphoric acid as the mobile phase at the flow rate of 1. 8 ml·min-1, and the sample size was 3 μl. Acid base titration method was used for measuring acid-neutralizing capacity. Results: No interference from the negative controls was shown to the TLC identification of Atractylodis macrocephalae Rhizoma. The fingerprint exhibited better separation of each peak. The precision, reproducibility and stability of the method were good,and the RSDs of the relative retention time and rela-tive peak area were less than 3. 0% . The linear range of paeoniflorin, tetrahydropalmatine and ammonium glycyrrhizinate was 0. 057-0. 568 μg(r=0. 999 9), 0. 035-0. 353 μg(r=0. 999 9)and 4. 244×10 -3-42. 44×10 -3μg(r=0. 999 9), respectively, and the av-eragerecoverywas99.3%(RSD=1.0%,n=6),100.0%(RSD=0.8%,n=6) and99.8%(RSD=1.2%,n=6),respectively. The average recovery of acid-neutralizing capacity was 99. 5% (RSD=0. 5% ,n=6). Conclusion: Exploratory research increases the specificity, controllability and safety of the standards, which provides reference for the further drug standards revision and the drug quality control.
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Objective:To develop a method of quantitative analysis of multi-components by single marker(QAMS)for the determi-nation of five constituents(ephedrine hydrochloride,amygdalin,liquiritin, baicalin and ammonium glycyrrhizinate)in Xiao'er Magan granule. Methods:Amygdalin was used as the internal reference substance, and the relative correlation factors(RCF) of ephedrine hydrochloride,liquiritin,baicalin and ammonium glycyrrhizinate to amygdalin were calculated and evaluated. The contents of the five constituents were determined by the external standard method(ESM) and QAMS,respectively. The content results determined by the two methods were compared and the feasibility of QAMS method was verified. Results:The RCF between amygdalin and the other con-tents was 1.237,1.318,1.327 and 0.884,respectively. There were no significant differences in the results between QAMS and ESM with the relative errors less than 0.3%. Conclusion:The QAMS method is accurate and feasible for the simultaneous determination of Xiao'er Magan granule.
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Objective: To establish an HPLC method for the simultaneous determination of five active components (paeoniflorin, liquiritin, ammonium glycyrrhizinate, edomin and osthole)in Pifukang lotion with multiple UV wavelengths.Methods: A Diamonsil C18 (200 mm×4.6 mm,5 μm) column was used with the mobile phase consisting of 0.1% hydrochloric acid and acetonitrile with gradient elution.The flow rate was 1.5 ml·min-1, and the column temperature was 30℃.Paeoniflorin was detected at 232 nm(0-6 min), liquiritin was detected at 277 nm(6-10 min),and ammonium glycyrrhizinate, edomin and osthole were detected at 254 nm(after 10 min).Results: The linear range of paeoniflorin,liquiritin,ammonium glycyrrhizinate, edomin and osthole was 28.200-282.000 μg·mL-1(r=0.999 7),12.150-121.500 μg·ml-1(r=0.998 8),13.420-134.200 μg·ml-1(r=0.999 5),0.047-0.466 μg·ml-1(r=0.999 9) and 2.38-23.8 μg·ml-1(r=0.999 9), respectively.The average recovery (RSD) was 98.49%(0.71%), 99.00%(0.62%), 98.38%(0.85%), 97.36%(0.92%) and 97.70%(0.78%), respectively (n=6).Conclusion: The established method is simple, accurate, highly sensitive and well reproducible, which can be used for the determination of the five active ingredients in Pifukang lotion.
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Objective:To establish the quality standard for two effective components in extractum glycyrrhizae capsules. Methods:Radix glycyrrhizae was identified by a TLC method. The contents of liquiritin and ammonium glycyrrhizinate in extractum glycyrrhizae capsules were determined by HPLC. An Inertsil C18 (150 mm × 4. 6 mm, 5μm) column was used. The mobile phase consisted of ace-tonitrile (A)-0. 2％ phosphoric acid (B) (0-8 min: 20％A-20％A;8-34 min: 20％A-50％A;34-35 min: 50％A-100％A;35-40 min:100％A-20％A) at a flow rate of 1. 0 ml·min-1 . The detection wavelength was at 237 nm under 25℃. Results: The spots in TLC were clear. Liquiritin showed a good linear relationship within the range of 0. 0020-0. 1000 mg·ml-1(r=0. 9995). The aver-age recovery was 100. 29％, and the RSD was 2. 94％(n=6). Ammonium glycyrrhizinate showed a good linear relationship within the range of 0. 0020-0. 1000 mg·ml-1(r=0. 9998). The average recovery was 101. 46％, and the RSD was 2. 33％(n=6). Conclu-sion:The method is simple,reliable and reproducible, which can be used for the quality control of the preparation.
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OBJECTIVE:To establish a method for simultaneous determination of paeoniflorin,berberine hydrochloride and ammonium glycyrrhizinate in Xiaoer huadu powder.METHODS:HPLC method was adopted.The separation was performed on Waters SunFireTM-C18 column with mobile phase consisted of acetonitrile-0.1％ phosphoric acid (gradient elution) at the flow rate of 1.0 mL/min.The detection wavelength was set at 238 nm,and column temperature was 25 ℃.The sample size was 10 μL.RESULTS:The linear ranges of paeoniflorin,berberine hydrochloride and ammonium glycyrrhizinate were 8.808-88.08 μg/mL(r=0.999 8),1.778-17.78 μg/mL(r=0.999 6),2.533-25.33 μg/mL(r=0.999 9),respectively.LOQ were 4.404,0.889,2.533 μg/mL;LOD were 1.101,0.445,1.267 μg/mL.RSDs of precision,stability and reproducibility tests were all lower than 2％.The recoveries were 95.08％-99.61％ (RSD=1.77％,n =9),96.93％-99.94％ (RSD=0.92％,n=9),98.33％-102.05％ (RSD=1.27％,n=9).CONCLUSIONS:The method is simple,accurate and reproducible,and can be used for simultaneous determination of paeoniflorin,berberine hydrochloride and ammonium glycyrrhizinate in Xiaoer huadu powder.
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OBJECTIVE:To develop a method for simultaneous determination of chlorogenic acid,geniposide,gentiopicro-side,ferulic acid,baicalin and ammonium glycyrrhizinate in Yindan pinggan capsule. METHODS:HPLC method was adopted. The separation was performed on Wonda SilTM-C18 column with mobile phase consisting of acetonitrile-0.4% phosphoric acid solu-tion(gradient elution)at the flow rate of 0.8 mL/min. The detection wavelength were set at 325 nm(chlorogenic acid,ferulic ac-id),250 nm (geniposide,ammonium glycyrrhizinate) and 275 nm (gentiopicroside,baicalin). The column temperature was 30 ℃. RESULTS:The linear ranges were 0.087-3.480 μg for chlorogenic acid(r=0.9998),0.201-8.040 μg for geniposide(r=0.9997),0.200-8.000 μg for gentiopicroside(r=0.9995),0.016-0.640 μg for ferulic acid(r=0.9999),0.105-4.200 μg for ba-icalin (r=0.9999) and 0.028-1.120 μg for ammonium glycyrrhizinate (r=0.9995),respectively. The limits of quantitation were 1.31,0.75,1.14,1.25,0.94,0.98 ng,and the limits of detection were 0.87,0.67,0.96,0.93,0.60,0.88 ng,respectively. RSDs of precision,stability and reproducibility tests were lower than 2.0%;recoveries were 99.9%-101.9%(RSD=0.7%,n=6), 98.7%-100.9%(RSD=0.9%,n=6),98.1%-101.5%(RSD=1.4%,n=6),98.5%-101.3%(RSD=1.3%,n=6),98.5%-101.7%(RSD=1.2%,n=6),98.2%-101.4%(RSD=1.2%,n=6),respectively. CONCLUSIONS:The method is simple and accurate , can be used for simultaneous determination of chlorogenic acid,geniposide,gentiopicroside,ferulic acid,baicalin and ammonium glycyrrhizinate in Yindan pinggan capsule.
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Objective: To develop an HPLC-DAD method for the simultaneous determination of liquiritin, ammonium glycyrrhizinate, vitexicarpin, pulegone, ferulic acid, chlorogenic acid, 3,5-dicaffeoyl quinic acid, berberine hydrochloride, kaempferol, and buddleoside in Boyun Tuiyi Pill (BTP). Methods: Shim-pack VP-ODS C18 column (250 mm × 4.6 mm, 5 μm) was adopted. The mobile phase was composed of methanol-acetonitrile (50:50, A) and 0.05% phosphoric acid (B) with gradient elution. Gradient elution: 0-5.0 min, 50% A; 5.0-30.0 min, 50%-80% A; 30.0-32.0 min, 80%-50% A; and 32.0-40.0 min, 50% A; Injection volume was 10 μL. The flow rate was 1.0 mL/min and the column temperature was 40℃. Results: liquiritin, ammonium glycyrrhizinate, vitexicarpin, pulegone, ferulic acid, chlorogenic acid, 3,5-dicaffeoyl quinic acid, berberine hydrochloride, kaempferol, and buddleoside were separated well. The linear calibration curves were obtained in 2-20 μg/mL for liquiritin, r = 0.999 2; 20-200 μg/mL for ammonium glycyrrhizinate, r = 0.999 5; 3-30 μg/mL for vitexicarpin, r = 0.999 4; 2-20 μg/mL for pulegone, r = 0.999 7; 1.2-12.0 μg/mL for ferulic acid, r = 0.999 5; 3.5-35.0 μg/mL for chlorogenic acid, r = 0.999 2; 8-80 μg/mL for 3,5-dicaffeoyl quinic acid, r = 0.999 3; 9-90 μg/mL for berberine hydrochloride, r = 0.999 3; 2-20 μg/mL for kaempferol, r = 0.999 6; and 3-30 μg/mL for buddleoside, r = 0.999 5. The average recoveries of the 10 constituents were 99.1%, 101.1%, 100.2%, 99.4%, 101.9%, 98.5%, 100.5%, 101.7%, 100.8%, and 99.7% with RSD of 0.62%, 0.79%, 0.77%, 0.83%, 0.47%, 0.38%, 0.97%, 1.05%, 0.86%, and 1.11%. The contents of six batches of the liquiritin, ammonium glycyrrhizinate, vitexicarpin, pulegone, ferulic acid, chlorogenic acid, 3,5-dicaffeoyl quinic acid, berberine hydrochloride, kaempferol, and buddleoside were 0.505-0.685, 1.793-2.012, 0.227-0.268, 0.183-0.206, 1.258-1.324, 0.348-0.381, 0.648-0.720, 1.544-1.722, 1.543-1.627, and 3.434-3.883 mg/pill, respectively. Conclusion: The method is rapid and has high sensitivity, high accuracy, and good specificity. It can be applied to the quality control of BTP.
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Objective: To establish an HPLC method for the simultaneous determination of catalpol, liquiritin, ammonium glycyrrhizinate, asarinin, verbascoside, atractylodin, ferulic acid, imperatorin, notopterol, isoimperatorin, baicalin, prim-O-glucosylcimifugin, and 5-O-methylvisammioside in Jiuwei Qianghuo Oral Liquid (JQOL). Methods: The analysis was performed on Zorbax Eclipse XDB-C18 column (250 mm×4.6 mm, 5 μm) by gradient elution of acetonitrile-0.005 mol/L KH2PO4 (adjusting to pH 3.0 with phosphoric acid) (15:85). The flow rate was 1.0 mL/min. Results: The linear ranges of catalpol, liquiritin, ammonium glycyrrhizinate, asarinin, verbascoside, atractylodin, ferulic acid, imperatorin, notopterol, isoimperatorin, baicalin, prim-O-glucosylcimifugin, and 5-O-methylvisammioside were 2.08-31.22 μg/mL (r=0.9995), 4.01-60.15 μg/mL (r=0.9992), 10.09-151.31 μg/mL (r=0.9992), 4.98-74.63 μg/mL (r=0.9994), 2.05-30.74 μg/mL (r=0.9996), 4.10-61.46 μg/mL (r=0.9996), 2.93-43.98 μg/mL (r=0.9993), 2.04-30.66 μg/mL (r=0.9995), 12.54-181.55 μg/mL (r=0.9997), 53.95-89.23 μg/mL (r=0.9995), 12.05-180.68 μg/mL (r=0.9995), 5.97-89.51 μg/mL (r=0.9994), and 7.99-119.82 μg/mL (r=0.9996). The average recoveries (n=6) were 98.8% (RSD=1.9%), 98.6% (RSD=1.8%), 101.2% (RSD=1.5%), 99.4% (RSD=0.8%), 100.1% (RSD=0.6%), 99.7% (RSD=0.9%), 98.9% (RSD=1.2%), 99.4% (RSD=2.0%), 100.5% (RSD=1.6%), 98.7% (RSD=0.8%), 101.2% (RSD=1.4%), 98.3% (RSD=1.5%), and 99.1% (RSD=1.7%), respectively. The contents of nine batches of the catalpol, liquiritin, ammonium glycyrrhizinate, asarinin, verbascoside, atractylodin, ferulic acid, imperatorin, notopterol, isoimperatorin, baicalin, prim-O-glucosylcimifugin, and 5-O-methylvisammioside were 0.229-0.259 mg/L, 1.231-1.260 mg/L, 0.849-0.877 mg/L, 0.357-0.371 mg/L, 0.149-0.169 mg/L, 0.941-0.967 mg/L, 0.529-0.547 mg/L, 0.269-0.294 mg/L, 1.039-1.067 mg/L, 0.043-0.064 mg/L, 3.631-3.649 mg/L, 0.157-0.183 mg/L, and 0.068-0.084 mg/L. Conclusion: This method is simple and rapid, and can be used for the quality control of JQOL with satisfactory separation and repeatability.
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Objective: To establish a reverse phase high performance liquid chromatographic (RP-HPL) method for the simultaneous determination of the contents of hastatoside, verbenalin, polydatin, ofrsytlloside A, verbascoside, ammonium glycyrrhizinate, and emodin in Shufeng Jiedu Capsule. Methods: RP-HPLC method was applied with the chromatographic condition as follows: the chromatographic column was Unitary C18 column (200 mm × 4.6 mm, 5 μm), acetonitrile-0.1% formic acid as the mobile phrase with gradient elution, the flow rate was 1.0 mL/min, the detection wavelength was 250 nm, the column temperature was 30℃, and the injection volume was 10 μL. Results: Linearity relationships of hastatoside, verbenalin, polydatin, ofrsytlloside A, verbascoside, ammonium glycyrrhizinate, and emodin were 0.096-1.920, 0.089-1.784, 0.119-2.348, 0.059-1.176, 0.021-4.224, 0.206-4.120, and 0.053-1.064 μg, respectively, as well as the average recoveries of 98.43% (RSD 2.13%), 98.30% (RSD 2.68%), 99.31% (RSD 2.76%), 101.64% (RSD 2.37%), 97.47% (RSD 2.05%), 100.89% (RSD 1.98%), and 99.05% (RSD 2.21%). Conclusion: The method is simple, fast, accurate, and can be used to control the quality of Shufeng Jiedu Capsule.
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Objective: To establish a new method for the quality evaluation of Shenxiong Yangxin Granule by fingerprint and quantitative analysis of multi-components by single marker method (QAMS) and validate its accuracy and feasibility for the application in preparation. Methods: The quality evaluation method was established and validated with was selected as markers of ingredients to HPLC fingerprint was established with Shenxiong Yangxin Granule as study object and puerarin as internal reference to determine the contents of other components (ferulic acid, hesperidin, salvianolic acid B, ammonium glycyrrhizinate, and schisandrin) according to the relative correction factor. The accuracy and feasibility of QAMS was evaluated by comparison on the results between the measured value and calculation value by external standard method and QAMS. Results: Seventeen common peaks were identified in the HPLC characteristic fingerprint, six components were verified in ten batches of Shenxiong Yangxin Granule, good similarities with correlation coefficients higher than 0.99 were found in the fingerprints. There was no significant difference between the quantitative results of the six ingredients in the ten batches by external standard method and QAMS. Conclusion: The method of fingerprint combined with QAMS has been verified in Shenxiong Yangxin Granule, which could be used as a reference for the quality control of multiple components determination and fingerprint chromatography for Shenxiong Yangxin Granule in future.
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Objective To establish a RP-HPLC method for determination of ammonium glycyrrhizinate in Shufei Mixture .Methods The sample was analyzed on an Agilent Zorbax SB-C18 column (4.6mm ×150 mm, 5μm), and acetonitrile-0.0025 mol/L sodium heptanesulfonate solution–0.05 mol/L potassium dihydrogen phosphate solution(20:45:45) ( adjusted pH value of 7.2 ±0.05 with 20% sodium hydroxide solution) was used as mobile phase.The flow rate was at 1.0 mL/min.The detective wavelength was at 250 nm.The column temperature was 30 ℃.Results With this chromatographic condition, the ammonium glycyrrhizinate peak in Shufei Mixture sample chromatogram could be separated with other ingredient peaks completely.The negative sample had no interference.The calibration curve was linear at a ranges of 23.6-118.1μg/mL for ammonium glycyrrhizinate, and equation of regression was Y=0.1133X–0.00110,r=0.999 8.The average recovery from sample was 97.8% and RSD was 0.88%(n=6).The content range of ammonium glycyrrhizinate in three batch Shufei Mixture sample was 0.2532-0.2865 mg/mL, and average content was 0.2721 mg/mL. Conclusion This method is simple, accurate, and useful for control method of this preparation.
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OBJECTIVE: To determine and compare the contents of principal component and related substances of ammonium glycyrrhizinate by methods contained in different pharmacopoeias and a new method established by our lab. METHODS: The methods for quality control of ammonium glycyrrhizinate in the latest edition of European Pharmacopoeia, British Pharmacopoeia, national drug standards of China, and the method established by our laboratory were employed to determine the contents of the principal component isomers and related substances of ammonium glycyrrhizinate in its raw materials and pharmaceutical products. The methods were evaluated and compared regarding the chromatographic features, resolution of principal component isomers, experimental cost, content determination results, and the advantages and disadvantages of each method were discussed. RESULTS: The mobile phases adopted in aforementioned pharmacopoeias are all acidic, which could not effectively separate 18α-glycyrrhizinic acid and 18β-glycyrrhizinic acid, thus could not truly reflect the contents of 18α-glycyrrhizinic acid, 18β-glycyrrhizinic acid, related substances A, and the related substances in the raw materials and pharmaceutical products. The resolution of principal component isomer by our method was 1.5, complying to the pharmacopoeia requirement. The content determination results of ammonium glycyrrhizinate raw materials by the four methods had no significant difference. CONCLUSION: Among the four methods, the method established by our laboratory performed best in terms of accuracy and practicability. This method has shorter detection time, lower cost, reduced toxicity and pollution, and the results are accurate and reliable, which suggests that it can be used for the chiral resolution of 18α-glycyrrhizinic acid and 18β-glycyrrhizinic acid and the content determination of principal component and related substances of the raw material and pharmaceutical products of ammonium glycyrrhizinate. This study provideds reference for further revision of the quality control method in Pharmacopoeia.
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Objective: To establish a new method for quantitative analysis on multi-components by single marker (QAMS) and validate its feasibility and technical adaptability in analysis on Shuangqing Yanhou Tablets (SYTs) for the simultaneous determination of 10 main constituents (citric acid, gallic acid, neochlorogenic acid, chlorogenic acid, cryptochlorogenic acid, isochlorogenic acid B, isochlorogenic acid A, isochlorogenic acid C, ammonium glycyrrhizinate, and artemisia ketone). Methods: Using SYTs as objects and the above 10 constituents as indexes, three correction methods were used to establish the relative correction factor (fk/s) between each component and gallic acid, respectively then to calculate the amount of each component and finally to achieve QAMS. At the same time, the external reference method and regression equation method were used to determine the amounts of the above 10 constituents, to compare the difference between the calculated and real data of the three fk/s, and to validate the correctness and adaptability of QAMS. Results: No significant difference was found in the quantitative results of 10 active constituents in three batches of SYTs determined by the calculated and real data. Conclusion: The QAMS by three correction methods is feasible and accurate to evaluate the contents of the 10 constituents in SYTs.
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AIM:To study the influence of material and configuration of microfiltration membranes on preparation of mono-ammonium glycyrrhizinate liposome(MGL) by membrane extrusion. METHODS: MGL were preparated by conventional rotary-evaporated film dispersion method and sonication,and MGL were extruding through 9 kinds of microfiltration membranes with 3 kinds of aperture specs of 0.1,0.2,0.45 ?m.The methods were evaluated by the filtration efficiency and the leakage rate of drug from liposomes. RESULTS: MGL were easily extruding through microfiltration membranes of NY6,PTFE,PVDF,PP and PC.MGL could not extruding through microfiltration membranes of PES,CN,CA and CA-CN.MGL become hardly to extrude through microfiltration membranes when increasing in the concentration of liposomes or the content of cholesterol.The leakage rate of drug from MGL was small when extruding through microfiltration membranes. CONCLUSION: The material and configuration of microfiltration membranes can remarkably influence the preparation of MGL by membrane extrusion method,and PC microfiltration membrane was selected.
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AIM: To establish quality standard for Compound Shengui Capsules. METHODS: Glycyrrhiza uralensis Fisch.、Panax notoginseng(Burk.) F.H.Chen、Salvia miltiorrhiza Bge.and Ligusticum chuanxiong Hort.were identified by TLC.Ammonium glycyrrhizinate and tanshinoneⅡ_A were determined by HPLC.(RESULTS): (TLC) spots developed were fairly clear and the blank test showed no interference.The linear rangers were 0.5-4?g(r=0.999 8)for ammonium glycyrrhizinate;0.04-0.32?g(r=0.999 6) for tanshinoneⅡ_A.The average recoveries of them were 98.9%,97.8%,respectively. CONCLUSION: The methods is effective for the quality control of Compound Shengui Capsules.