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1.
China Pharmacy ; (12): 26-31, 2022.
Article in Chinese | WPRIM | ID: wpr-907008

ABSTRACT

OBJECTIVE To improve the quality standard of T ibetan medicine of Qinjiaohua ,and to provide scientific basis for comprehensive quality evaluation. METHODS The qualitative analysis of 16 batches of Qinjiaohua with different producing areas and different origins was carried out by microscopic and TLC identification. According to the method stated in 2020 edition of Chinese Pharmacopoeia ,water content ,total ash content ,acid-insoluble ash content and alcohol-soluble extract content were determined. HPLC method was used to determine the contents of 5 components (loganic acid ,swertiamarin,gentiopicrin, swertionolin,isoorientin) in Qinjiaohua. RESULTS The medicinal powder of Qinjiaohua was light brown-yellow ,and the microscopic features of the powder were clear ,and pollen grains ,ducts,non-glandular hairs ,corolla epidermal cells and calyx epidermal cells were all found. The results of TLC indentification showed that there were fluorescent spots of the same color in the chromatogram of the tested product and the corresponding position of substance control (isoorientin). The content ranges of water content,total ash content ,acid-insoluble ash content and alcohol-soluble extract were 5.40%-8.87%,3.76%-6.40%,0.27%-0.58%, 26.81%-42.51%,respectively. The results of content determination methodology met the requirements of pharmacopoeia ;the content ranges of loganic acid ,swertiamarin,gentiopicrin,swertionolin and isoorientin in 16 batches of Qinjiaohua were 3.13-9.36,1.26-22.39,13.80-74.60,1.24-12.22,2.58-14.96 mg/g,respectively. CONCLUSIONS On the basis of the original quality standard of Qinjiaohua ,microscopic identification ,TLC identification ,content determination and examination items of water,total ash ,acid-insoluble ash and alcohol-soluble extract are added. It is preliminarily proposed that water content ,total ash content and acid-insoluble ash content should not exceed 9.0%,6.5% and 0.6%,while the contents of ethanol-soluble extract and gentiopicrin should not be less than 26.0% and 13.8 mg/g,respectively.

2.
Article in Chinese | WPRIM | ID: wpr-923030

ABSTRACT

Objective To revise the determination method in the quality standard of Jingtian Zhitong cream. Methods The total saponins of angelica sinensis, Ligusticum wallichii, Rhizoma corydalis, and Panax notoginseng saponins were qualitatively identified by thin-layer chromatography (TLC). The contents of notoginsenoside R1, ginsenoside Rg1, and ginsenoside Rb1 in the preparation were determined by high performance liquid chromatography (HPLC). Results TLC showed strong specificity and good resolution. The concentration of notoginsenoside R1 showed a good linear relationship in the range of 0.1604 and 2.0050μg (r=0. 999). The concentration of ginsenoside Rg1 showed a good linear relationship in the range of 0.8003 and 10.0035μg (r=1.000). The concentration of ginsenoside Rb1 showed good linearity in the range of 0.6182 and 7.7275μg (r=1.000). The sample recovery rates were 101.43%, 98.75% and 100.95%, respectively. The relative standard deviation (RSD) were 2.56%, 2.71% and 2.75%, respectively. Conclusion The developed method is accurate and reliable with high sensitivity, which can be used for the quality control of Jingtian Zhitong cream.

3.
Article in Chinese | WPRIM | ID: wpr-923029

ABSTRACT

Objective To improve the quality standards of Kunxian capsules (KC) and effectively control the product quality. Methods Triptolide, icariin and hypericin were used as the indicator components, to increase or improve the thin layer chromatography (TLC) identification methods of Kunming begonia, epimedium and dodder. Agilent ZORBA SB-C18 (4.6 mm×250 mm, 5 μm) as a chromatographic column, the HPLC method for the determination of triptolide was improved with acetonitrile-0.1% formic acid solution as the mobile phase and 220 nm as the detection wavelength. Results The spots in the TLC method of Kunming begonia, epimedium and dodder has strong specificity, good and clear separation of characteristic spots, negative and no interference. The quantitative analysis of the content of triptolide in KC showed that there is a good linear relationship (r=0.9995) between the mass concentration of triptolide and the peak area in the range of 40.16-502.00 μg/ml, the average recovery was 98.12%, RSD was 8.25%, and the accuracy was good. Conclusion The TLC identification method and HPLC method established in this experiment have strong specificity and good reproducibility, and can effectively control the quality of KC.

4.
Article in Chinese | WPRIM | ID: wpr-888141

ABSTRACT

In view of the current inadequate standards for Gleditsiae Spina in the Chinese Pharmacopoeia, this study put forward some new items of the quality standards of Gleditsiae Spina. Thin-layer chromatography(TLC) was performed for identification with the reference substance of taxifolin and the reference material of Gleditsiae Spina as the control. According to the general principles of the Chinese Pharmacopoeia(2020 edition, Vol. 4), the moisture, total ash content, and alcohol-soluble extract of medicinal materials and decoction pieces of Gleditsiae Spina were determined. The content determination method for medicinal materials and decoction pieces of Gleditsiae Spina was established using high-performance liquid chromatography(HPLC), with taxifolin as the quality control index. Based on the determination results of 30 batches of samples of Gleditsiae Spina from different habitats, the draft quality standards of Gleditsiae Spina were developed, which provided suggestions for the revision of the quality standards of Gleditsiae Spina in the Chinese Pharmacopoeia.


Subject(s)
Chromatography, High Pressure Liquid , Drugs, Chinese Herbal , Quality Control , Reference Standards
5.
China Pharmacy ; (12): 1949-1955, 2021.
Article in Chinese | WPRIM | ID: wpr-886577

ABSTRACT

OBJECTIVE:To provide scientifi c evidence for improving the quality standard of Mongolian medicine Juniperus rigida. METHODS :Totally 10 batches of J. rigida from different places were taken as samples to observe their characters and identify them by microscope ;TLC method was adopted to qualitatively identify isoquercitrin ,quercitrin,amentoflavone, podocarpusflavone A and hinokiflavone ;the contents of total ash ,acid-insoluble ash ,ethanol-soluble extract and heavy metals were determined by related method stated in 2020 edition of Chinese Pharmacopeia (part Ⅳ). The contents of above 5 components in samples were determined by HPLC. RESULTS :The powder of J. rigida was green or yellowish green ,polygonal tracheids , closely arranged in longitudinal with unequal stomatal ;epidermal cells were nearly rectangular ;sclerenchyma cells were quasi rectangular and the wall beadedly thickening. Results of TLC showed that the spots of the same color were found in the corresponding positions of chromatogram for test sample and substance control. The contents of total ash ,acid-insoluble ash and ethanol-soluble extract in 10 batches of samples were 7.37%-11.18%,0.75%-2.98%,16.55%-26.42%,respectively;average contents were 8.51%,1.27%,22.35%. The contents of lead ,arsenic,cadmium,mercury and copper were 2.00-5.44,0.65-1.65, 0.044-0.100,0.034-0.160,4.59-6.79 mg/kg,respectively;average conte nts were 3.73,0.97,0.078,0.061,5.23 mg/kg. The linear ranges of isoquercitrin ,quercitrin,amentoflavone,podocarpus- flavone A and hinokiflavone were 4.98-20.02,49.99-199.96, 19.94-99.96,9.99-40.00,20.20-159.98 μg/mL(all r>0.999 7); com RSDs of precision ,repeatability and stability (24 h) tests were all less than 3.00%(n=6);the average recoveries were 话:0993-2057878。E-mail:Tanghuishz@qq.com 100.62%-102.96%,RSDs were 1.21%-1.88%(n=6). Average contents of the above-mentioned 5 compounds in 10 batches of samples were 0.089-0.379,1.379-4.250,1.077-2.026,0.162-0.423, 0.016 9-0.117 0 mg/g,respectively. CONCLUSIONS :The qualitative and quantitative analysis methods of Mongolian medicine J. rigida are established. It is preliminarily proposed that the total ash content shall not exceed 10.22%,the acid-insoluble ash content shall not exceed 1.53%,ethanol-soluble extract content shall not be less than 17.88%,heavy metal lead should not exceed 5 mg/kg,arsenic should not exceed 2 mg/kg,cadmium should not exceed 0.3 mg/kg,mercury should not exceed 0.2 mg/kg,copper should not exceed 20 mg/kg.

6.
Acta Pharmaceutica Sinica B ; (6): 203-221, 2021.
Article in English | WPRIM | ID: wpr-881133

ABSTRACT

@#New Delhi metallo-β-lactamase-1 (NDM-1) is capable of hydrolyzing nearly all β-lactam antibiotics, posing an emerging threat to public health. There are currently less effective treatment options for treating NDM-1 positive “superbug”, and no promising NDM-1 inhibitors were used in clinical practice. In this study, structure–activity relationship based on thiosemicarbazone derivatives was systematically characterized and their potential activities combined with meropenem (MEM) were evaluated. Compounds 19bg and 19bh exhibited excellent activity against 10 NDM-positive isolate clinical isolates in reversing MEM resistance. Further studies demonstrated compounds 19bg and 19bh were uncompetitive NDM-1 inhibitors with Ki = 0.63 and 0.44 μmol/L, respectively. Molecular docking speculated that compounds 19bg and 19bh were most likely to bind in the allosteric pocket which would affect the catalytic effect of NDM-1 on the substrate meropenem. Toxicity evaluation experiment showed that no hemolysis activities even at concentrations of 1000 mg/mL against red blood cells. In vivo experimental results showed combination of MEM and compound 19bh was markedly effective in treating infections caused by NDM-1 positive strain and prolonging the survival time of sepsis mice. Our finding showed that compound 19bh might be a promising lead in developing new inhibitor to treat NDM-1 producing superbug.

7.
Acta Pharmaceutica Sinica B ; (6): 156-180, 2021.
Article in English | WPRIM | ID: wpr-881131

ABSTRACT

@#This study was aimed to design the first dual-target small-molecule inhibitor co-targeting poly (ADP-ribose) polymerase-1 (PARP1) and bromodomain containing protein 4 (BRD4), which had important cross relation in the global network of breast cancer, reflecting the synthetic lethal effect. A series of new BRD4 and PARP1 dual-target inhibitors were discovered and synthesized by fragment-based combinatorial screening and activity assays that together led to the chemical optimization. Among these compounds, 19d was selected and exhibited micromole enzymatic potencies against BRD4 and PARP1, respectively. Compound 19d was further shown to efficiently modulate the expression of BRD4 and PARP1. Subsequently, compound 19d was found to induce breast cancer cell apoptosis and stimulate cell cycle arrest at G1 phase. Following pharmacokinetic studies, compound 19d showed its antitumor activity in breast cancer susceptibility gene 1/2 (BRCA1/2) wild-type MDA-MB-468 and MCF-7 xenograft models without apparent toxicity and loss of body weight. These results together demonstrated that a highly potent dual-targeted inhibitor was successfully synthesized and indicated that co-targeting of BRD4 and PARP1 based on the concept of synthetic lethality would be a promising therapeutic strategy for breast cancer.

8.
Article in Chinese | WPRIM | ID: wpr-862491

ABSTRACT

Objective To improve the quality control of Dilong Shenmai oral liquid. Methods TLC was used for the qualitative identification of Astragali Radix, Ophiopogonis Radix and Schisandrae Chinensis Fructus in Dilong Shenmai oral liquid. HPLC was used to determine the contents of schisandrin and ethylparaben in the preparation. Wondasil C18 column (250 mm×4.6 mm, 5 μm) was used with acetonitrile-water as the mobile phase at the flow rate of 1.0 ml/min for gradient elution. The detection wavelength was set at 254 nm, and column temperature was 30 ℃. Results TLC spots were clear and well-separated without negative interference. The linear ranges of schisandrin and ethylparaben were 5.81−58.06 μg/ml (r=0.999 9) and 25.29−252.94 μg/ml (r=0.999 9). The average recoveries were 99.35% (RSD=1.02%) and 99.72% (RSD=0.76%). Conclusion This method is simple, quick and accurate. It can be used for effective quality control of Dilong Shenmai oral liquid.

9.
China Pharmacy ; (12): 536-541, 2021.
Article in Chinese | WPRIM | ID: wpr-873665

ABSTRACT

OBJECTIVE:To improve the quality standard of M ongolian med icine Artemisia sacrorum ,and to provide scientific basis for comprehensive quality evaluation. METHODS :The appearance and microscopic characteristics of A. sacrorum were identified;scopoletin,chlorogenic acid ,caffeic acid ,scopoletin and 3,5-dicaffeoylquinic acid were identified quantitatively by TLC;the contents of above 5 components were determined by HPLC. The water content ,total ash and extract were examined. RESULTS:The stem of A. sacrorum was cylindrical ,and its surface was purple or purple-brown or cyan-brown ;the leaves were ovate or oblong-ovate ,fragrant;the flowers were yellow ,head-shaped,subglobose or hemispherical. The powder was green or yellow-green,its pollen grain had three germination ;the parenchymal cell clusters with sharp edges and numerous threaded ducts , occasionally having marginal pitted ducts ;its wood fibers were in bundles mostly. Results of TLC showed that the spots of the same color were found in the corresponding positions of chromatogram for 5 substance control and samples. The linear range of scopoletin, chlorogenic acid , caffeic acid , scopolactone and 3,5-dicaffeoylquinic acid were 85.60-428.00, 10.16-101.60, 10.20-102.00,40.84-408.40 and 40.80-408.00 μg/mL(all r>0.999 0). RSDs of precision ,stability,repeatability tests were all less than 3.00%(n=6). The average recoveries were 103.07%,99.66%,98.37%,97.78%,98.40%(all RSDs <3.00%,n=6). The contents of the above-mentioned 5 compounds in 10 batches of samples were 0.36%-1.23%,0.09%-0.51%,0.04%-0.13%, 0.61% -1.13% ,0.12% -1.11% ,respectively;the average com contents of water ,total ash and water soluble extract were 6.25%,5.86%,26.50%,respectively. CONCLU SIONS:O the basis of the original quality standard of A. sacrorum , microscopic identification,TLC identification ,content determination and examination items of water ,total ash and extract are added. The method shows good precision ,accuracy and stability ,which can provide reference for more scientific and standardized evaluation of the quality of this medicinal material.

10.
Acta Pharmaceutica Sinica B ; (6): 2709-2718, 2021.
Article in English | WPRIM | ID: wpr-888882

ABSTRACT

Protein arginine methyltransferases (PRMTs) have been implicated in the progression of many diseases. Understanding substrate recognition and specificity of individual PRMT would facilitate the discovery of selective inhibitors towards future drug discovery. Herein, we reported the design and synthesis of bisubstrate analogues for PRMTs that incorporate a

11.
Rev. colomb. quím. (Bogotá) ; 49(2): 18-22, mayo-ago. 2020. tab, graf
Article in English | LILACS-Express | LILACS | ID: biblio-1115658

ABSTRACT

Abstract The objective of this study was to identify the emetic metabolites in different parts of the P. ipecacuanha, a plant with emetic properties. Partial phytochemical analysis was performed to determine the presence of emetine and cephaeline in leaves, stems and roots. Both alkaloids were detected in the three plant parts analyzed. Highest alkaloid content was found in roots (8.55 mg/g), followed by stems (4.05 mg/g), and the lowest was found in leaves (2.4 mg/g). The cephaeline content (8.35 mg/g) was higher than that of emetine (6.65 mg/g) in all the three organs analyzed. Toxicity analysis of the crude extract showed a LD50 of 500 mg/kg.


Resumen El objetivo de este estudio fue identificar los metabolitos eméticos en diferentes partes de P.ipecacuanha, una planta con propiedades eméticas. Se realizó un análisis fitoquímico parcial, donde se determinó la presencia de emetina y cefalina en hojas, tallos y raíces. Ambos alcaloides se detectaron en las tres partes de la planta analizadas. El mayor contenido de alcaloides se encontró en las raíces (8.55 mg/g), seguido de los tallos (4.05 mg /g), y el más bajo se encontró en las hojas (2.4 mg/g). El contenido de cefalina (8,35 mg/g) fue mayor que el de emetina (6,65 mg/g) en los tres órganos analizados. El análisis de toxicidad del extracto crudo mostró una DL50 de 500 mg/kg.


Resumo O objetivo deste estudo foi identificar os metabólitos eméticos em diferentes partes do P. ipecacuanha, uma planta com propriedades eméticas. Foi realizada análise fitoquímica parcial para determinar a presença de emetina e cefelina nas folhas, caules e raízes. Ambos os alcalóides foram detectados nas três partes da planta analisadas. O maior teor de alcalóides foi encontrado nas raízes (8,55 mg/g), seguido dos caules (4,05 mg/g), e o menor foi encontrado nas folhas (2,4 mg/g). O conteúdo de cefhaelina (8,35 mg/g) foi superior ao de emetina (6,65 mg/g) nos três órgãos analisados. A análise de toxicidade do extrato bruto mostrou um LD50 de 500 mg/kg.

12.
Article | IMSEAR | ID: sea-212461

ABSTRACT

Background: Recovery after surgery for patients with colorectal disease has improved with the advent of minimal access surgery and standardized recovery protocols. Despite these advances, anastomotic leakage remains one of the most dreaded complications following colorectal surgery, with rates of 3-27 per cent depending on specific risk factors. The aim of the study was to assess sensitivity and specificity of systemic and peritoneal drain-fluid bio-markers in early prediction of anastomotic leak; and to co-relate rise in levels of biomarkers and severity of clinical symptoms in patients who have undergone colo-rectal surgeries.Methods: The present study was a prospective observational study conducted on 60 patients in the Postgraduate Department of Surgery, Government Medical College, Srinagar after obtaining due ethical clearance over a period of two years.Results: The mean age was 54.87±11.901 years with 44 patients (73.3%) were males. Among systemic makers: the mean CRP level was 2.7800±0.500 mg/L, the mean total leukocyte count was 10.783±0.940 thousands and the mean serum procalcitonin level was 0.365±0.1385 ng/ml. Among peritoneal fluid drain bio-makers, the mean IL-6 level was 3551.066±1311.965 pg/ml, the mean IL-10 level was 628.533±460.358 pg/ml and the mean TNF-a level was 16.391±6.736 pg/ml. The anastomotic leak after colo-rectal surgery was noted in 16 patients (26.7%). In our study significant co-relation was noted between the rise in levels of peritoneal drain fluid biomarkers and severity of clinical symptoms but no significant co-relation was noted between the rise in levels of systemic markers and severity of clinical symptoms in patients who have undergone colo-rectal surgeries.Conclusions: Systemic biomarkers are poor predictors of anastomotic leak after colorectal surgery. But sensitivity and specificity of peritoneal fluid drain biomarkers in predicting anastomotic leak was significantly high.

13.
Article | IMSEAR | ID: sea-212974

ABSTRACT

Primary omental infarction (POI) is a rare cause of acute abdomen. It frequently mimics other causes of acute abdomen. It is being diagnosed more frequently with the advancement of radiology. Here we report a case of a 35 years old man admitted in emergency with pain right side abdomen since past 2 days. On physical examination patient was febrile with tenderness and guarding over right side of abdomen, TLC (total leucocyte count) - 13.2×109/l, mild rise in bilirubin with rest blood investigations being normal. CT (computed tomography) abdomen was s/o omental infarction. On diagnostic laparoscopy gangrenous omentum with torsion over a vascular pedicle was noted, omentectomy was performed laparoscopically. In conclusion omental infarction should be kept as a differential diagnosis in acute abdomen especially right-side abdominal pathologies. It can be managed conservatively but if signs of sepsis are there it is wise to perform a diagnostic laparoscopy.

14.
Article | IMSEAR | ID: sea-211011

ABSTRACT

Normal concentration of WBCs in blood varies between 4000 and 11,000 per microliter and are classified intotwo variants namely granulocytes and agranulocytes on the basis of presence and absence of granules.Manual methods of calculation of TLC include- Neubauer chamber and estimating WBC on leishman stainedslides whereas automated methods are based on impedance or light scattering technology. The study comparedthe efficacy of both these methods in statistical terms using Chi Square test. 100 cases of leucocytosisanalyzed over a period of 1 year at MMIMSR, Mullana, Haryana revealed leucocytosis prevalent in 4-6 decadeof life with slight male predominance. The pearson coefficient for TLC came out to be p value =0.215 (notsignificant) but for DLC, calculations revealed p values for polymorphs, lymphocytes, eosinophils andmonocytes to be significant (p value =0.000 each). To conclude, standard manual methods should be advocatedas special practice where there is definite need of morphological and quantitative evaluation of WBCs and tovalidate the automated methods by which the laboratories can optimize patient care and not as a replacement

15.
Chinese Pharmaceutical Journal ; (24): 357-361, 2020.
Article in Chinese | WPRIM | ID: wpr-857764

ABSTRACT

OBJECTIVE: To establish the TLC identification and HPLC quantitative analysis method of Artemisia ordosica. METHODS: TLC and HPLC were used for qualitative and quantitative analysis of A. ordosica collected from five different regions. The TLC conditions were as follows: the reference substance was spathulenol, the adsorbent was silica gel G, the developing agent was petroleum ether (60-90 ℃)-acetone (5∶1) and the chromogenic color reagent was alcoholic solution of sulfuric acid (10%). The reference substance was 5,4′-dihydroxy-7-methoxyflavanone, the adsorbent was silica gel G, the developing agent was dichloromethane-ethyl acetate-formic acid (15∶1∶0.1) and the chromogenic reagent was ultraviolet lamp. The HPLC separation was set at performed on Topsil C18 (4.6 mm×250 mm,5 μm); the mobile phase was composed of water (A) and acetonitrile (B) and the gradient elution program was as follows: 0-15 min,25%-38% B;15-40 min,38%-45% B. The detection wavelength was 275 nm with column temperature kept at 30 ℃. RESULTS: The spots of reference substances (spathulenol and 5,4′-dihydroxy-7-methoxyflavanone) and A. ordosica in TLC had good repeatability and were easy to be identified. Under the HPLC conditions adopted in this study, all calibration curves exhibited good linearity (r>0.999 3). The recoveries of the method were 97.75%, 96.00%, 98.20%, 97.00%, 95.50%, 99.33%, 97.50%, 96.50%, and 97.33%, respectively. The RSDs were less than 2.0%. Compounds 1, 2, 5 and 8 were not detected in some samples, while compounds 3, 4, 6, 7 and 9 were detected and their content changes in different samples were (0.998±0.013)-(1.263±0.018), (0.108±0.002)-(0.301±0.005), (1.201±0.018)-(1.457±0.023), (0.635±0.011)-(0.801±0.013), (1.150±0.018)-(1.222±0.023) mg•g-1, respectively. CONCLUSION: The TLC identification and HPLC quantitative analysis of A. ordosica are established and can be used for the quality control of A. ordosica.

16.
Chinese Pharmaceutical Journal ; (24): 465-472, 2020.
Article in Chinese | WPRIM | ID: wpr-857756

ABSTRACT

OBJECTIVE: To optimize and improve the quality standard of Qingkailing dropping pills. METHODS Lonicerae Japonicae Flos, geniposide in Gardeniae Fructus and baicalin in Scutellariae Radix of Qingkailing dropping pills were identified by TLC and HPLC respectively. Cholic acid and hydrodeoxycholic acid were determined by HPLC equipped with an ELSD and a column (4.6 mm×250 mm, 5 μm) packed with ODS bonded silica gel (5 μm particle size). The mobile phase was a mixture of methanol, acetonitrile and 0.1% formic acid (68∶17∶15, V/V/V) and the flow rate was 1.0 mL•min-1. Geniposide in Gardeniae Fructus of Qingkailing dropping pills was determined by HPLC equipped with a DAD (238 nm) and a column (4.6 mm×250 mm) packed with ODS bonded silica gel (5 μm particle size). The mobile phase was a mixture of acetonitrile and 0.05% phosphoric acid (10∶90, V/V) and the flow rate was 1.0 mL•min-1. Baicalin in Scutellariae Radix of Qingkailing dropping pills was determined by HPLC equipped with a DAD (275 nm) and a column (4.6 mm×150 mm) packed with ODS bonded silica gel (5 μm particle size), the mobile phase was a mixture of methnol, water and phosphoric acid (47∶53∶0.2, V/V/V), and the flow rate was 1.0 mL•min-1. RESULTS: The developed TLC spots were clear with good reproducibility. Hydrodeoxycholic acid, cholic acid, geniposide and baicalin showed good linear relationship in the ranges of 0.505 0-6.312 μg, 0.515-6.440 μg, 0.029 12-0.582 4 μg, and 0.109 2-1.092 μg, respectively. The average recoveries (n=6) were 101.5%, 101.6%, 98.61% and 99.77%, with RSDs of 1.7%, 1.5%, 1.42% and 0.79%, respectively. CONCLUSION: The method is simple, rapid, accurate, with low toxicity, and can be used to control the quality of Qingkailing dropping pills more effectively and comprehensively.

17.
Article in Chinese | WPRIM | ID: wpr-846233

ABSTRACT

Objective: To establish a scientific and reasonable quality control method of Bufei Granules through the qualitative and quantitative research of thin layer identification and content determination of Bufei Granules. Methods: Based on the main chemical constituents of each drug in Bufei Granules, TLC method was used to analyze Corni Fructus, Ephedrae Herba, Paeoniae Radix Rubra, Scutellariae Radix, Citri Reticulatae Pericarpium, and Glycyrrhizae Radix et Rhizoma; HPLC was used to determine the content of loganin and baicalin. The content of loganin was analyzed by Agilent Eclipse XDB-C18 column (250 mm × 4.6 mm, 5 μm) with the mobile phase of acetonitrile-methanol-water-formic acid (10:1:89:0.1). The detection wavelength was set at 236 nm; The content of baicalin was analyzed by Dikma Diamonsil C18 column (250 mm × 4.6 mm, 5 μm) with the mobile phase of methanol-water-formic acid (49:51:0.1). The detection wavelength was set at 280 nm. Results: The TLC identification method can distinguish Ephedrae Herba, Paeoniae Radix Rubra, Scutellariae Radix, Citri Reticulatae Pericarpium, and Glycyrrhizae Radix et Rhizoma with clear spots, no negative interference, good separation and strong specificity. Loganin and baicalin were used as index components in methodological study. The average recovery of loganin was 98.49% and the RSD was 0.80%; The repeatability test RSD was 0.83% which met the requirement. The linear range was from 4.76 μg/mL to 50.70 μg/mL and the linear relationship was good (r = 0.999 9). The average recovery of baicalinrate was 101.20% and the RSD was 0.77%. The repeatability test RSD was 0.90%, which met the requirements. The linear range was from 6.00 μg/mL to 96.00 μg/mL and the linear relationship was good (r = 0.999 9). The loganin content of three bantches of samples was 12.04, 9.78 and 11.81 mg/bag; And the content determination result of baicalin was 121.13, 101.31 and 103.14 mg/bag. Conclusion: The method is easy to operate, strong in specificity, accurate and sensitive, with good repeatability. It can be applied for the quality control of Bufei Granules.

18.
China Pharmacy ; (12): 2230-2234, 2020.
Article in Chinese | WPRIM | ID: wpr-825653

ABSTRACT

OBJECTIVE:To establish the quality standards of Mongolian medicine Cynanchum thesioides. METHODS :TLC was used for the qualitative identification of C. thesioides . According to 2015 edition of Chinese Pharmacopeia (part Ⅳ),the moisture,total ash and ethanol-soluble extract were determined. HPLC method was used to determine the content of thesioideoside in C. thesioides . RESULTS :TLC spots were clear ,there were same yellow green fluorescent spots on the corresponding position of the sample (C. thesioides )and control (thesioideoside). In 22 batches of samples ,contents of moisture were 6.18%-12.97%,total ash were 4.64%-7.95%,ethanol-soluble extract were 12.46%-32.70%. The linear range of thesioideoside were 0.048-3.050 μg(R2= 0.999 9). RSDs of precision , stability, repeatability and durability tests were all less than 1% . The recoveries were 104.03%-106.36%(RSD=0.96%,n=6). The contents of thesioideoside in 22 batches of C. thesioides were 0.006 2%-0.130 5%. CONCLUSIONS:It is suggested that the moisture and total ash should not exceed 11.50% and 7.50%,respectively;the contents of ethanol-soluble extract and the sioideoside are no less than 17.00% and 0.05%,respectively. The established quality standards can be used for quality control of Mongolian medicine C. thesioides .

19.
China Pharmacy ; (12): 2106-2111, 2020.
Article in Chinese | WPRIM | ID: wpr-825190

ABSTRACT

OBJECTIVE:To improve the quality standard of Compound child antifebrile suppository. METHODS :Based on the previous quality standard ,TLC identification methods were established for artificial cow-bezoar and Baphicacanthis Cusiae Rhizoma et Radix. HPLC method was established for content determination of choleic acid (CA),hyodeoxycholic acid (HDCA) and paracetamol. RESULTS :TLC chromatogram of artificial cow-bezoar and Baphicacanthis Cusiae Rhizoma et Radix all showed the same color spots in the same position as the corresponding substance control or reference medicinal material ,while the negative samples had no interference. HPLC was performed on Welch Xtimate C 18 column(CA,HDCA)or Agilent ZORBAX SB-C 18 column(paracetamol)with mobile phase consisted of acetonitrile-0.5% formic acetic acid (by gradient elution ,CA and HDCA )or methanol-water(20∶80,V/V,paracetamol)at the flow rate of 1.0 mL/min. ELSD was used with a nitrogen flow-rate of 2.0 L/min at a drift tube temperature of 105 ℃(CA,HDCA). The detection wavelength was set at 244 nm(paracetamol). The linear ranges of CA,HDCA,paracetamol were 0.150 0-4.500 0,0.212 5-6.375 0,0.081 9-1.638 5 μg(all r>0.999 2). RSDs of precision , reproducibility and stability tests were all lower than 3%(n=6 or n=7). The average recoveries were 100.35%,101.39%, 98.81%(all RSD <3%,n=6). CONCLUSIONS :Based on previous quality standard of Compound child antifebrile suppository , TLC method is used to identify artificial cow-bezoar and Baphicacanthis Cusiae Rhizoma et Radix ,and the contents of CA ,HDCA and paracetamol are determined by HPLC ,which can effectively improve the quality control standard of the preparation.

20.
China Pharmacy ; (12): 1080-1085, 2020.
Article in Chinese | WPRIM | ID: wpr-821497

ABSTRACT

OBJECTIVE:To provide reference for improving the quality sta ndard of Equisetum hyemale . METHODS :Totally 10 batches of E. hyemale from different sites were collected as samples. TLC method was used to qualitatively identify kaempferol- 3-O-β-sophoroside. The contents of heavy metal ,aflatoxin,impurity,moisture,total ash ,acid-insoluble ash ,water-soluble extract and ethanol-soluble extract were determined according to supplementary provisions of Chinese Pharmacopoeia (2015 edition). HPLC method was used to determine the content of kaempferol- 3-O-β-sophoroside in sample. HPLC fingerprint of water-soluble extract from E. hyemale was also established. RESULTS :TLC identification showed that in the chromatogram of the test sample , fluorescent spots with the same color were displayed on the corresponding positions of the chromatogram of substance control of kaempferol-3-O-β-sophoroside,and without interference from blank control. Among 10 batches of samples ,the contents of impurities were 0.19%-2.32%;the water contents were 10.12%-11.87%;the total ash contents were 6.67%-10.11%;the acid-insoluble ash contents were 1.34%-2.12%;the water-soluble extract contents were 9.17%-13.99%;the ethanol-soluble extract contents were 7.49%-13.68%,respectively. It is preliminarily proposed that the impurity content shall not exceed 3.00%;the total ash content shall not exceed 10.00%;the acid-insoluble ash content shall not exceed 2.50%;the water-soluble extract content shall not be less than 9.00% ;the ethanol-soluble extract content shall not be less than 5.00%. Arsenic(0.064-0.225 mg/kg) 010815) was detected in 9 batches of samples ;cadmium(0.106-0.132 E-mail:cruise0303@163.com mg/kg)was detected in 6 batches of samples ;lead(0.221- 1.896 mg/kg)was detected in all samples ,but no mercury or rebecca aflatoxin was detected. The results of HPLC method met the relevant requirements of Chinese Pharmacopoeia . The content of kaempferol- 3-O-β-D-sophoroside in 10 batches of samples was 627.12-5 384.53 mg/kg,and the similarity of HPLC fingerprints of 10 batches of samples was more than 0.900. CONCLUSIONS : A new qualitative and quantitative analysis method for kaempferol- 3-O-β-D-sophoroside was established ;the heavy metals , aflatoxins,impurities and other items in E. hyemale were detected ;the limits of impurity ,ash and extract were determined. The established method is simple ,accurate and reproducible ,and can be used for quality control of E. hyemale .

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