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Objective: To establish the HPLC fingerprint and simultaneously determinate nine components of the standard decoction of Wenjing Decoction, so as to provide reference for the quality control of Wenjing Decoction of classical prescriptions. Methods: Fingerprints of 15 batches of the standard decoction of Wenjing Decoction were determined by HPLC-PDA, and the control fingerprint was established. All samples were analyzed by Kromasil C18 chromatographic column (250 mm × 4.6 mm, 5 μm) maintained at 25 ℃, and eluted with acetonitrile-0.1% phosphoric acid at the flow rate of 0.8 mL/min, and the detection wavelength was 220, 280, 320 and 380 nm respectively. Combined with cluster analysis (CA), principal component analysis (PCA), and partial least squares discriminant analysis (PLS-DA), the quality of 15 batches of Wenjing Decoction was analyzed. At the same time, the contents of nine active components were determined. Results: The similarity of 15 batches of standard decoction of Wenjing Decoction was between 0.902 and 0.992, and a total of 18 common peaks were identified and nine of them (2-gallic acid, 5-paeoniflorin, 7-liquiritin, 8-ferulic acid, 9-isoliquiritin apioside, 11-isoliquiritin, 14-cinnamaldehyde, 15-ammonium glycyrrhetate, 16-paeonol) were quantitative analyzed. CA, PCA and PLS-DA were used to classify the 15 batches of samples into two groups. The results of quantitative analysis were good, and the recovery rate of nine components was 94.91%-108.16%. The content of gallic acid, paeoniflorin, iquiritin, ferulic acid, isoliquiritin apioside, isoliquiritin, cinnamaldehyde, ammonium glycyrrhetate, paeonol in 15 batches of samples were in the range of 10.7-31.3, 95.8-228.4, 18.6-62.4, 3.3-8.3, 4.8-18.7, 2.8-10.6, 13.7-108.2, 83.9-292.3, and 31.1-125.5 mg/g, respectively. Conclusion: The HPLC fingerprint combined with the simultaneous determination of multicomponent analysis method eatablished in this experiment are stable and reliable, which can provide the theoretical guidance for the quality evaluation of Wenjing Decoction and its compound preparations.
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OBJECTIVE： To develop a method for simultaneous determination of 7 components of Niuhuang qingwei pills as chlorogenic acid， geniposide， forsythoside A， narirutin， baicalin， ammonium glycyrrhetate， chrysophanol. METHODS： HPLC-wavelength switching method was adopted. The determination was performed on Agilent ZORBAX SB-C18 column with mobile phase consisted of acetonitrile （A）-0.1％ phosphoric acid （B） gradient elution at the flow rate of 1.0 mL/min. The detection wavelengths were set at 348 nm （chlorogenic acid）， 238 nm （geniposide）， 330 nm （forsythoside A）， 280 nm （narirutin and baicalin）， 237 nm （ammonium glycyrrhetate）， 254 nm （chrysophanol）. The column temperature was 30 ℃， and sample size was 10 μL. RESULTS： The linear ranges of chlorogenic acid， geniposide， forsythoside A， narirutin， baicalin， ammonium glycyrrhetate， chrysophanol were 0.011 67-0.233 4 μg （r＝0.999 4）， 0.042 91-0.858 1 μg （r＝0.999 4）， 0.125 0-2.500 μg （r＝0.999 9）， 0.118 0- 2.360 μg （r＝0.999 9）， 0.119 6-2.392 μg （r＝0.999 7）， 0.030 57-0.611 4 μg （r＝0.999 6）， 0.006 201-0.124 0 μg（r＝0.999 4）， respectively； the limits of quantitation were 1.167， 0.858， 1.250， 1.180， 1.196， 0.611， 0.620 μg/mL， respectively； RSDs of precision tests were 0.98％， 1.04％， 0.59％， 1.50％， 0.83％， 1.24％ and 1.32％ （n＝6）， respectively. RSDs of stability tests were 1.21％， 0.97％， 1.42％， 0.71％， 0.98％， 1.87％ and 1.63％ （n＝6， 12 h）， respectively. Average recoveries were 98.32％， 98.11％， 98.81％， 98.50％， 98.30％， 98.16％ and 97.83％， and the RSDs were 1.37％， 1.41％， 0.64％， 1.01％， 1.18％， 1.16％ and 1.16％ （n＝6）， respectively. CONCLUSIONS： Established method is easy and reproducible. It can be used for the quality control of Niuhuang qingwei pills.
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To establish a determination method for the contents of ammonium glycyrrhetate,nardosinone,and curcumin in transdermal receptor liquid of Baimai Ointment,and investigate the percutaneous permeability of Baimai Ointment and the effects of two kinds of penetration enhancers on percutaneous absorption of three components. The contents of ammonium glycyrrhetate,nardosinone,and curcumin in transdermal receptor liquid were determined by high pressure liquid chromatography( HPLC). The vertical modified Franz diffusion cell was used to perform a transdermal experiment in vitro with the abdominal skin of mice( treated and untreated). The transdermal receptor liquid was preferably used to investigate the transdermal absorption rule of the Baimai Ointment and the effect of the penetration enhancer. The results showed that the comprehensive solubility of PEG-ET-NS( 3 ∶3 ∶4) was best among three types of receptor liquid PG-ET-NS( 3 ∶3 ∶4),PEG-ET-NS( 3 ∶3 ∶4),ET-NS( 3 ∶7). PEG-ET-NS was used as the receptor liquid for in vitro transdermal experiments. The cumulative permeation area of ammonium glycyrrhetate,nardosinone and curcumin within 24 h was 5. 73,18. 99,0. 38 μg·cm~(-2)respectively. Taking QEFand ER as comprehensive evaluation indicators of permeation performance,the comprehensive penetration-promoting performance of ammonium glycyrrhizinate: 3% PEG 400-ethanol-normal saline ≈ 1. 19 times( 3%azone) = 1. 94 times( blank); comprehensive penetration-promoting performance of nardosinone: 3% PEG 400-ethanol-normal saline≈1. 28 times( 3% azone) = 1. 37 times( blank); the comprehensive penetration performance of curcumin: 3% PEG 400-ethanol-normal saline≈1. 77 times( 3% azone) ≈3. 42 times( blank). The comprehensive penetration enhancement properties of the two penetration enhancers were as follows: 3% PEG 400-ethanol-normal saline>3%azone>blank. The transdermal absorption curve of ammonium glycyrrhetate,nardosinone and curcumin in Baimai Ointment were consistent with the zero-order equation,indicating that the transdermal absorption process was irrelevant to the concentration of three components,and its was a diffusion process. This experiment provides reference for the study of ointment transdermal preparations.
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Animais , Camundongos , Administração Cutânea , Pomadas , Farmacocinética , Permeabilidade , Pele , Absorção CutâneaRESUMO
OBJECTIVE:To compare in vitro percutaneous permeation characteristics of glycyrrhizic acid in 6 kinds of glycyrrhetate creams,and to provide reference for further development and utilization. METHODS:Modified Franz diffusion cell and isolated rat skin were adopted for in vitro percutaneous permeation test. 24 h accumulative permeation of glycyrrhizic acid in 6 kinds of glycyrrhetate creams(monoammonium glycyrrhizinate,diammonium glycyrrhizinate,monopotassium glycyrrhizinate, dipotassium glycyrrhizate,trisodium glycyrrhizinate,disodium glycyrrhetate)were determined by HPLC. The permeation characteristics of 6 kinds of glycyrrhetate creams were evaluated by calculating percutaneous absorption rate. RESULTS:24 h accumulative permeation of 6 kinds of glycyrrhetate in rat skin in descending order was as follows:trisodium glycyrrhizinate (23.933 μ g/cm2)>dipotassium glycyrrhizinate(22.952 μ g/cm2)>disodium glycyrrhizinate(15.424 μ g/cm2)>monopotassium glycyrrhizinate(10.703 μg/cm2)>diammonium glycyrrhizinate(9.557 μg/cm2)>monoammonium glycyrrhizinate(1.621 μg/cm2). The percutaneous permeation rate in descending order was as follows as trisodium glycyrrhizinate [1.010 2 μ g/(cm2·h)]>dipotassium glycyrrhizinate [0.974 5 μg/(cm2·h)]>disodium glycyrrhizinate [0.641 2 μg/(cm2·h)]>diammonium glycyrrhizinate [0.399 9 μg/(cm2·h)]>monopotassium glycyrrhizinate[0.362 8 μg/(cm2·h)]>monoammonium glycyrrhizinate[0.072 6 μg/(cm2·h)]. CONCLUSIONS:The permeation rate of trisodium glycyrrhizinate is the highest among 6 kinds of glycyrrhetate creams in vitro.
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OBJECTIVE:To establish the method for simultaneous determination of gallic acid,rosmarinic acid,liquiritin and ammonium glycyrrhetate in Regan saibisitan granules. METHODS:RP-HPLC method was adopted. The determination was per-formed on Waters RP-C18 column with mobile phase consisted of acetonitrile-0.2% phosphoric acid (gradient elution) at the flow rate of 1.0 mL/min. The detection wavelengths were 210 nm(gallic acid,rosmarinic acid and liquiritin),230 nm(ammonium glyc-yrrhetate). The column temperature was 28 ℃,and sample size was 20 μL. RESULTS:The linear ranges were 0.2744-7.546 μg for gallic acid(r=0.9998),0.1870-5.143 μg for rosmarinic acid(r=0.9996),0.1300-3.575 μg for liquiritin(r=0.9999)and 0.2540-6.985μg for ammonium glycyrrhetate(r=0.9998),respectively. The LOQ were 2.67,1.36,1.09 and 2.11 ng,respective-ly. The LOD were 1.03,0.62,0.87 and 0.91 ng,respectively. RSDs of precision,stability and repeatability tests were all less than 2.0%. The average recoveries were 97.26%-101.00%(RSD=1.1%,n=9),97.66%-101.80%(RSD=1.3%,n=9),97.45%-101.70%(RSD=1.4%,n=9),97.74%-101.70%(RSD=1.4%,n=9). CONCLUSIONS:The method is simple,accurate and reproducible, and can be applied for simultaneous determination of gallic acid,rosmarinic acid,liquiritin and ammonium glycyrrhetate in Regan saibisitan granules.
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Objective: To develop a UPLC-MS/MS method for simultaneously determining harpagide, liquiritin, harpagoside, platycodin D, ammonium glycyrrhetate, ophiopogonin D, methylophiopogonanone A, and methylophiopogonanone B in Xuanmai Ganjie Granules (composed with Scrophulariae Radix, Ophiopogonis Radix, Glycyrrhizae Radix et Rhizoma, and Platycodonis Radix) from different pharmaceutical companies. Methods: The chromatographic separation was achieved on Phenomenex Kenetix C18 column (50 mm × 2.1 mm, 5 μm) by using a mobile phase consisted of acetonitrile and 0.1% formic acid water at the flow rate of 0.3 mL/min for gradient elution. Simultaneous monitoring of positive and negative ions and multiple reaction monitoring (MRM) scan mode were applied to the quantification of the components in Xuanmai Ganjie Granules; Sample volume was 5 μL. Results: There was good linearity between the absorption peak area and the concentration for harpagide, liquiritin, harpagoside, platycodin D, ammonium glycyrrhetate, ophiopogonin D, methylophiopogonanone A, and methylophiopogonanone B in the ranges of 9-2250, 8-2000, 3.4-850, 96-24000, 12.4-3100, 3.6-1900, 1.7-425, and 1.5-375 ng/mL, respectively. The average recoveries were ranged from 97.2% to 102.8% (RSD ≤ 2.7%). The contents of harpagide, liquiritin, harpagoside, platycodin D, ammonium glycyrrhetate, ophiopogonin D, methylophiopogonanone A, and methylophiopogonanone B in eight batches of samples were in the ranges of 32.8-107.6, 54.8-178.0, 14.6-70.7, 31.2-280.0, 106.4-287.9, 0.1-0.6, 0.01-0.07, and 0.03-0.17 μg/g, respectively. Conclusion: The developed method is simple, effective, and credible for determining the eight components in Xuanmai Ganjie Granules. It provides more helpful information for the comprehensive quality evaluation of Xuanmai Ganjie Granules.
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In this article, a method to determine the content of liquiritin, ammonium glycyrrhetate, costunolide and dehydrocostus lactone in Mongolia medicine Ga Ri Di-13 pill was established. The chromatographic condition for liquiritin and ammonium glycyrrhetate was listed as the below: with Dimma column (250 mm×4.6 mm, 5μm) as stationary phase; with acetonitrile (A)-0.4%phosphoric acid (B) as mobile phase; gradient elution: 0-10 min (16%-18% A), 10-30 min (18% A), 30-40 min (18%-27% A), 40-85 min (27%-45% A), and 85-86 min (45%-16%A); column temperature was set at 30℃; detection wavelength was 237 nm; and flow velocity was 1 mL·min-1. The chromatographic column condition for costunalide and dehydrocostus lactone was listed as the below: with Dimma column (250 mm×4.6 mm, 5μm) as stationary phase; with acetonitrile-water (65:35) as mobile phase; detection wavelength was 225 nm; column temperature was set at 30℃ and flow velocity was 1.0 mL·min-1. The linearity ranges of liquiritin, ammonium glycyrrhetate, costunolide, and dehydrocostus lactone were 0.1-1.2μg (r=0.999 9), 0.341-4.092μg (r=1.000 0), 0.12-1.2μg (r=1.000 0), and 0.106-1.06 (r=1.000 0), respectively; the average recovery rates were 97.07%, 100.13%, 98.44%, and 98.90%, respectively; the RSD were 1.00%, 1.84%, 2.21% and 3.38%,respectively. This method is specificity and reproducible, and can be used to determination of liquiritin, ammonium glycyrrhetate, costunolide and dehydrocostus lactone in Mongolia medicine Ga Ri Di -13 pill.
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Objective To establish the standard for quality control ofQingyan Granule. Methods The chief components of the preparation, Sophora Tonkinensis radix et rhizoma, Adenophorae radix, Lonicera japonica caulis, and Ophiopogonis radix were identified by TLC qualitatively. The contents of licorice glycosides and glycyrrhizic acid were determined by HPLC. The separation was performed on Thermo Syncronis C18 column (4.6 mm×250 mm, 5μm) with mobile phase consisted of acetonitrile with 0.05% phosphoric acid solution (A)-0.05% phosphoric acid solution (B), and gradient elution (0-8 min, 19%A;8-35 min, 19%→50%A). Detection wavelength was 237 nm, and flow rate was 1 mL/min.Results The spots in TLC were clear. There were spots with same color on the corresponding location of reference substance and reference herbal, negative control without interference. The linear range for licorice glycosides was 0.05-0.5μg (r=0.999 9). The average recovery was 99.97%, RSD=1.74% (n=9). The linear range for glycyrrhizic acid was 0.1-2μg (r=0.999 9). The average recovery was 99.74%, RSD=1.28% (n=9). Conclusion The method is simple, accurate, with high reproducibility, which can be used for quality control ofQingyan Granule.
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Objective:To develop a method to determine benzalkonium chloride in compound aspartate, vitamin B6 and dipotassi-umglycyrrhetateeyedrops.Methods:TheseparationwasperformedonanAgilentZorbaxC18(150mm×4.6mm,5μm)column. The mobile phase consisted of acetonitrile-5 mmol·L-1 ammonium acetate ( in which 1% triethylamine was added, then the pH value was adjusted to 5. 0 ± 0. 5 by acetic acid) 65∶35(v/v). The flow rate was 1. 0 ml·min-1 and the detection wavelength was 214nm. Re-sults:Benzalkonium chloride had a good linearity within the range of 50. 00-150. 00μg·ml-1(r=0. 998 0), and the average recovery was 99. 1%(RSD=0. 6%). Conclusion:The method is simple, rapid and sensitive with good repeatability and recovery. It can be used to determine benzalkoinum chloride in compound aspartate, vitamin B6 and dipotassium glycyrrhetate eye drops.
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Objective To investigate the therapeutic effect of chronic hepatitis treated by Magnesium Isoglycyrrhizinate injection.Methods Eighty chronic hepatitis patients were treated by Magnesium Isoglycyrrhizinate injection,ivgtt,150mg,qd.The control group were 80 chronic hepatitis patients treated by Diammonium Glycyrrhetate injection,ivgtt,150mg,qd.To observe therapeutic effect after four weeks treatment.Results The therapeutic effect rate in treatment group was 91.2％,excellence rate is 63.8％.There was significant difference between the two groups (64.2％,46.2％ all P ＜0.05).Conclusion Magnesium Isoglycyrrhizinate injection can effectively treat chronic hepatitis.
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Objective To compare the curative effect of magnesium isoglycyrrhizinate and compound ammonium glycyrrhetate in patients with liver cirrhosis of decompensated.Methods Eighty-six patients with liver cirrhosis of decompensated were enrolled into the study and randomly divided into two groups: the treatment group(n=43) were given magnesium isoglycyrrhizinate once a day in addition to routine treatment;the control group(n=43) were given compound ammonium glycyrrhetate once a day in addition to routine treatment.The clinical manifestation,including symptoms,signs and hepatic function were observed.The clinical lab data,including blood routine examination,urine routine test and kidney function of all patients from two groups were collected before and after the treatments.The adverse drug reactions were monitored throughout the whole therapy.Results ALT and AST turned to normal in 97.7%(42/43) and 90.7%(39/43) of patients respectively in the treatment group,which were significantly higher than those of 72.1%(31/43) and 74.4%(32/43) respectively in the control group( x2=9.86 and 4.73,respectively,Ps＜0.05). Time to turning to normal in ALT and AST were(21.6±9.1)d and(23.1±10.6)d in the treatment group,which were significantly lower than those of(37.5±17.8)d,and(46.7±19.4)d respectively in the control group(t=5.23 and 7.01,respectively,Ps＜0.01).Conclusion The results suggested that magnesium isoglycyrrhizinate had better effect on alleviating symptoms and decreasing enzyme in treatment of liver cirrhosis of decompensated stage.
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Objective To establish a HPLC method for the simultaneous determination of chlorogenic acid,liquiritigenin,cinnamic acid,and monoammonium glycyrrhetate in Tong Saimai Pellets.Methods A Zorbax 80A Extend-C18 column was used.The mobile phase consisted of acetonitrile and 0.1% phosphoric acid,and was used for gradient elution.Chlorogenic acid,liquiritigenin,cinnamic acid and monoammonium glycyrrhetate were determined by dual wavelength,?s=276nm,?R=590nm.Results The linear range of chlorogenic acid was 0.0505~1.6160 ?g,and r=0.9999;the average recovery was 98.17%,and sR=4.28%(N=6).The linear range of liquiritigenin was 0.0252~0.8064 ?g,and r=0.9999;the average recovery was 93.76%,and sR=1.94%(N=6).The linear range of cinnamic acid was 0.0111~0.3552?g,and r=0.9999;the average recovery was 98.25%,and sR =2.72%(N=6).The linear range of monoammonium glycyrrhetate was 0.3300~10.5600?g,and r=0.9999;the average recovery was 102.6%,and sR=1.93%(N=6).Conclusion This method is convenient,rapid and accurate,and it can be used for quality control of the production of Tong Saimai Pellets.