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ObjectiveTo improve the quality standard of Yuanhu Zhitong oral liquid in order to strengthen the quality control of this oral liquid. MethodThin layer chromatography(TLC) was used for the qualitative identification of Corydalis Rhizoma and Angelicae Dahuricae Radix in Yuanhu Zhitong oral liquid by taking tetrahydropalmatine, corydaline reference substances and Corydalis Rhizoma reference medicinal materials as reference, and cyclohexane-trichloromethane-methanol(5∶3∶0.5) as developing solvent, Corydalis Rhizoma was identified using GF254 glass thin layer plate under ultraviolet light(365 nm). And taking petroleum ether(60-90 ℃) -ether-formic acid(10∶10∶1) as developing solvent, Angelicae Dahuricae Radix was identified using a silica gel G TLC plate under ultraviolet light(305 nm). High performance liquid chromatography(HPLC) was performed on a Waters XSelect HSS T3 column(4.6 mm×250 mm, 5 μm) with acetonitrile(A)-0.1% glacial acetic acid solution(adjusted pH to 6.1 by triethylamine)(B) as the mobile phase for gradient elution(0-10 min, 20%-30%A; 10-25 min, 30%-40%A; 25-40 min, 40%-50%A; 40-60 min, 50%-60%A), the detection wavelength was set at 280 nm, then the fingerprint of Yuanhu Zhitong oral liquid was established, and the contents of tetrahydropalmatine and corydaline were determined. ResultIn the thin layer chromatograms, the corresponding spots of Yuanhu Zhitong oral liquid, the reference substances and reference medicinal materials were clear, with good separation and strong specificity. A total of 12 common peaks were identified in 10 batches of Yuanhu Zhitong oral liquid samples, and the peaks of berberine hydrochloride, dehydrocorydaline, glaucine, tetrahydropalmatine and corydaline. The similarities between the 10 batches of samples and the control fingerprint were all >0.90. The results of determination showed that the concentrations of corydaline and tetrahydropalmatine had good linearity with paek area in the range of 0.038 6-0.193 0, 0.034 0-0.170 0 g·L-1, respectively. The methodological investigation was qualified, and the contents of corydaline and tetrahydropalmatine in 10 batches of Yuanhu Zhitong oral liquid samples were 0.077 5-0.142 9、0.126 1-0.178 2 g·L-1, respectively. ConclusionThe established TLC, fingerprint and determination are simple, specific and reproducible, which can be used to improve the quality control standard of Yuanhu Zhitong oral liquid.
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Objective@#This study aimed to evaluate the nutritional adequacy and compliance with cardiovascular disease (CVD) guidelines in therapeutic diets implemented in four hospitals in General Santos City, Philippines. @*Methods@#The study employed a cross-sectional study and analyzed the one-day therapeutic menus of four hospitals using the Philippine Food Composition Table and the United States Department of Agriculture nutrient database. The nutrient contents calculated in this study were compared among hospitals and benchmarked against the Philippine Dietary Reference Intakes (PDRI) and CVD-specific guidelines, the Dietary Approaches to Stop Hypertension (DASH), and Therapeutic Lifestyle Changes (TLC). The nutrient adequacy ratios (NARs) and the corresponding mean (SD) values were used to interpret the data.
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Cardiovascular Diseasesالملخص
AIM To improve the quality standard for Guanxin Shengmai Pills.METHODS TLC was adopted in the qualitative identification of Ginseng Radix et Rhizoma and Notoginseng Radix et Rhizoma,the analysis was performed on a silica G thin layer plate,along with the low layer solution of chloroform-methanol-water(13 : 7 : 2)stood at below 10℃ as a mobile phase,and 10%sulfuric acid ethanol solution as a derivatization reagent.HPLC was applied to determining the contents of ginsenoside Rg1,ginsenoside Re,ginsenoside Rb1 and ginsenoside Rd,the analysis was performed on a 20℃ thermostatic Thermo Accucore-C18 column(4.6 mm×150 mm,2.6 μm),with the mobile phase comprising of acetonitrile-water flowing at 0.8 mL/min in a gradient elution manner,and the detection wavelength was set at 203 nm.RESULTS The clear TLC bands present without negative interference.Four constituents showed good linear relationships within their own ranges(R2≥0.999 9),whose average recoveries were 91.21%-106.86%with the RSDs of 0.68%-1.43%.CONCLUSION This specific and reproducible method can provide a reference for the quality control of Guanxin Shengmai Pills.
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Objective To study the quality standard of Gardenia jasminoides and its effective parts. Methods TLC was used to identify Gardenia jasminoides and its effective parts. The heavy metals, harmful elements, and moisture in Gardenia jasminoides and its effective parts were examined. The content of Gardenia jasminoides and its effective parts was determined by high performance liquid chromatography. Results TLC method could be used to identify Gardenia jasminoides and its effective parts. The moisture content of Gardenia jasminoides and its effective parts were 8.4% and 3.2%, respectively. ICP-MS was used to determine the contents of five elements in Gardenia jasminoides and its effective parts simultaneously. There was a good linear relationship between arsenic, cadmium, copper, mercury, and lead in the range of 0~20, 0~10, 0~500, 0~5 and 0~20 ng/ml, respectively; The method detection limit of each metal element was 3.3×10−5~1.3×10−3 mg/kg. The relative standard deviation (RSD) of precision was 0.32%~0.82%. RSD values of each element content showed that the method had good repeatability. And the recoveries of arsenic, cadmium, copper, mercury, and lead were 103%~112%, 98%~99%, 98%~99%, 105%~106% and 100%~103%, respectively (n=3). The stability of each element was good within 8 h. The contents of the five elements were within the limits of the current edition of Chinese Pharmacopoeia. The standard curve equation of gardenia was Y=15860X+22543, r=0.9999, indicating that there was a good linear relationship of gardenia in the range of 20.16~322.6 μg/ml. The RSD of precision was 1.86%. RSD of the two samples were 2.38% and 2.60%, respectively, indicated that the method had good repeatability. The average recovery of Gardenia was 99.1% (n=6). The stability of the two solutions was good within 8 h. The contents of gardenia and its effective parts were 5.71% and 34.2%, respectively. Conclusion The research on the quality of Gardenia jasminoides effective parts was carried out based on the research on the quality of Gardenia jasminoides, and the results met the requirements. Therefore, the method established in this experiment could control the quality of Gardenia jasminoides and its effective parts simultaneously.
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AIM To optimize the TLC identification method for Cirsii Herba and to study the changes in quality properties"carbonizing retains characteristics"of Cirsii Herba Carbonisata.METHODS After the improvement of thin layer plate and solvent in the TLC identification based on the Chinese Pharmacopoeia 2020 Edition for Cirsii Herba,Cirsii Herba Carbonisata had its TLC identification method and UPLC fingerprint established for the determination of its content of buddleoside and acacetin as well.RESULTS We used silica gel G plate,and the solvent of toluene-acetone-formic acid-methanol(6 ∶ 3 ∶ 0.5 ∶ 2.5)for TLC identification of Cirsii Herba.The content variations of buddleoside and acacetin in Cirsii Herba and its differently charred products were consistent with the result of the TLC identification.CONCLUSION The improved TLC identification method for Cirsii Herba is of lower cost and less solvent toxicity compared to the method in the Chinese Pharmacopoeia 2020 Edition,and can identify the changes in quality properties"carbonizing retains characteristics"of differently charred Cirsii Herba,therefore it can be used to control the quality of Cirsii Herba Carbonisata in the market.
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Objective The identification of Santali Albi Lignum and its common counterfeits Osyris lanceolata Lignum,Santalum spicatum Lignum was studied to provide experimental basis for the authenticity of this medicinal herb.Methods The identification was carried out using morphological,microscopic,and thin-layer identification methods.The volatile oil of Santali Albi Lignum and its counterfeits were extracted by steam distillation and the volatile oil components were analyzed by gas chromatography-mass spectrometry(GC-MS).The differences of volatile oil components among the three were compared.Results Santali Albi Lignum and its common counterfeits all possessed a sandalwood aroma,but Santali Albi Lignum has abundant oiliness and strong aroma.Osyris lanceolata Lignum aroma exhibits slightly strong odor and slightly camphor flavor,and the smell of Santalum spicatum Lignum is sweet and fragrant.Santali Albi Lignum is greyish-yellow to yellowish-brown in color,while Osyris lanceolata Lignum is generally reddish brown in color,Santalum spicatum Lignum is light yellow to light yellowish-brown,but its surface shows reddish-brown when exposed to air for a long time.In the transection section,the ray width of Santali Albi Lignum is more than 1-2 rows of cells,with occasional 3 rows of cells.The ray width of Osyris lanceolata Lignum is 1-3 rows of cells,while the ray width of Santalum spicatum Lignum is 1-2 rows of cells,mostly uniseriate.In the tangential section,the wood ray of Santali Albi Lignum has a height of 5-15 cells,the wood ray of Osyris lanceolata Lignum has a height of 4-10 cells,while the wood ray of Santalum spicatum Lignum has a height of 4-16 cells.In the radial section,fewer calcium oxalate crystal was found in Santali Albi Lignum,more calcium oxalate crystal was appeared in Osyris lanceolata Lignum,more and larger calcium oxalate crystal was identified in Santalum spicatum Lignum.Genuine and fake sandalwood can be distinguished using sandalwood oil as the thin-layer chromatographic reference.And the volatile oil content of fake Osyris lanceolata Lignum and Santalum spicatum Lignum is lower than that of Santali Albi Lignum.The main components of Santali Albi Lignum are α-santalol and β-santalol.The low content of santalol has been found in Osyris lanceolata Lignum,while α-santalol is extremely low in Santalum spicatum Lignum oil and β-santalol has not been found.Conclusion There are small differences among Santali Albi Lignum and its adulterants in characteristics,microscopical characteristics.But the differences have been found in three-way cross section,thin layer chromatography,volatile oil content and composition characteristics,which can be used for identification of Santali Albi Lignum and its counterfeits.
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ObjectiveTo establish the specific chromatogram and thin layer chromatography(TLC) of Qingxin Lianziyin(QXLZY) benchmark samples, in order to clarify the key quality attributes and provide a reference for the quality evaluation of QXLZY. MethodHigh performance liquid chromatography(HPLC) specific chromatogram of QXLZY benchmark samples was developed by using a YMC Hydrosphere C18 column(4.6 mm×250 mm, 5 μm) with the mobile phase of acetonitrile(A)-0.2% formic acid aqueous solution(B) for gradient elution(0-10 min, 5%-20%A; 10-20 min, 20%A; 20-25 min, 20%-24%A; 25-40 min, 24%-30%A; 40-55 min, 30%-50%A; 55-65 min, 50%-100%A; 65-75 min, 100%A; 75-75.1 min, 100%-5%A; 75.1-90 min, 5%A), and the detection wavelength was 360 nm. Ultra-high performance liquid chromatography-linear ion trap/orbitrap mass spectrometry(UHPLC-LTQ-Orbitrap MS) with electrospray ionization(ESI) was used to identify the components of QXLZY benchmark samples by accurate relative molecular weight and multilevel MS fragment ion information, the detection conditions were positive and negative ion modes and data dependency scanning mode. TLC identification methods for Ophiopogonis Radix, Lycii Cortex, Nelumbinis Semen, Poria, Astragali Radix and Ginseng Radix et Rhizoma in QXLZY were established. ResultA total of 15 characteristic peaks were identified from Glycyrrhizae Radix et Rhizoma, Plantaginis Semen and Scutellariae Radix, and the relative standard deviations of the retention times of 15 characteristic peaks in 15 batches of QXLZY benchmark samples were≤3% with peak 8(baicalin) as the reference peak. A total of 100 compounds, including flavonoids, organic acids, saponins, amino acids and others, were identified in the benchmark samples by UHPLC-LTQ-Orbitrap MS. The established TLC had good separation and was suitable for the identification of Ophiopogonis Radix, Lycii Cortex, Nelumbinis Semen, Poria, Astragali Radix and Ginseng Radix et Rhizoma in QXLZY. ConclusionThe material basis of QXLZY benchmark samples is basically determined by MS designation and source attribution. The established specific chromatogram and TLC of QXLZY are simple, stable and reproducible, which can provide a reference for the development and quality control of QXLZY.
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ObjectiveTo establish the specific chromatogram and thin layer chromatography(TLC) identification method of Kaixinsan(KXS) samples, in order to clarify the key quality attributes and provide reference for the quality evaluation of KXS. MethodHigh performance liquid chromatography(HPLC) specific chromatogram of KXS was developed with YMC Hydrosphere C18 column(4.6 mm×250 mm, 5 μm), the mobile phase was acetonitrile(A)-0.2% formic acid aqueous solution(B) for gradient elution(0-15 min, 2%-20%A; 15-25 min, 20%-25%A; 25-30 min, 25%-30%A; 30-45 min, 30%-31%A; 45-50 min, 31%-44%A; 50-65 min, 44%-45%A; 65-73 min, 45%-75%A; 73-95 min, 75%-100%A; 95-105 min, 100%A; 105-105.1 min, 100%-2%A; 105.1-120 min, 2%A), the detection wavelength was 320 nm. Ultra high performance liquid chromatography-linear ion trap-electrostatic field orbitrap mass spectrometry(UHPLC-LTQ-Orbitrap MS) was used to identify the chemical components of KXS with electrospray ionization(ESI), negative ion mode and scanning range of m/z 50-2 000. TLC identification methods for Poria and Ginseng Radix et Rhizoma in KXS were established. ResultThere were 11 common peaks in the specific chromatogram of KXS, attributed to Polygalae Radix, Poria and Acori Tatarinowii Rhizoma. Taking peak 9(α-asarone) as the reference peak, the relative standard deviations of the retention times of 15 batches of KXS samples were<0.2%. A total of 34 compounds were identified by UHPLC-LTQ-Orbitrap MS, including terpenoids, phenylpropanoids, oligosaccharides and ketones. The established TLC had good separation and was rapid, reliable, simple, feasible, suitable for the identification of Poria and Ginseng Radix et Rhizoma in KXS. ConclusionThe specific chromatogram and TLC of KXS are stable and reproducible. The material basis of KXS is basically clarified by MS, which can provide a reference for the development and quality control of KXS.
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ObjectiveTo establish the identification method of Dalbergiae Odoriferae Lignum(DOL) and its counterfeits by nuclear magnetic resonance hydrogen spectrum(1H-NMR) combined with multivariate statistical analysis. Method1H-NMR spectra of DOL and its counterfeits were obtained by NMR, and the full composition information was established and transformed into a data matrix, and the detection conditions were as follows:taking dimethyl sulfoxide-d6(DMSO-d6) containing 0.03% tetramethylsilane(TMS) as the solvent, the constant temperature at 298 K(1 K=-272.15 ℃), pulse interval of 1.00 s, spectrum width of 12 019.23 Hz, the scanning number of 16 times, and the sampling time of 1.08 s. Similarity examination and hierarchical cluster analysis(HCA) were performed on the data matrix of DOL and its counterfeits, and orthogonal partial least squares-discriminant analysis(OPLS-DA) was used to analyze the data matrix and identify the differential components between them. In the established OPLS-DA category variable value model, the category variable value of DOL was set as 1, and the category variable value of the counterfeits was set as 0, and the threshold was set as ±0.3, in order to identify the commercially available DOL. The OPLS-DA score plot was used to determine the types of counterfeits in commercially available DOL, and it was verified by thin layer chromatography(TLC). ResultThe results of similarity analysis and HCA showed that there was a significant difference between DOL and its counterfeits. OPLS-DA found that the differential component between DOL and its counterfeits was trans-nerolidol. The established category variable value model could successfully identify the authenticity of the commercially available DOL. The results of the OPLS-DA score plot showed that there were heartwood of Dalbergia pinnata and D. cochinchinensis in the commercially available DOL, and were consistent with the TLC verification results. ConclusionThere is a phenomenon that heartwood of D. pinnata and D. cochinchinensis are sold as DOL in the market. 1H-NMR combined with multivariate statistical analysis can effectively distinguish DOL and its counterfeits, which can provide a reference for the identification of them.
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Background: Neonatal sepsis is characterized by systemic signs and symptoms of generalised bacterial infection in the first four weeks of life. Early recognition and diagnosis of neonatal sepsis remains a challenge because of the variable and nonspecific clinical presentation. A combination of haematological and biochemical tests may provide a more rapid diagnosis of sepsis than blood culture which takes at least 24 to 48 hours for the results. Objectives: To study the correlation of parameters of sepsis screen with blood culture in neonates with clinical sepsis and or having significant risk factors for sepsis and To study the outcome of neonatal sepsis was our secondary aim.Material & Methods:The descriptive prospective study with cross sectional design was conducted on 100 neonates admitted with signs and symptoms of sepsis in the nursery ward and NICU of paediatric department of BebeNanki Hospital, GMC, Amritsar. Sepsis screen and blood culture (gold standard for neonatal sepsis diagnosis) and other relevant investigations were sent under strict aseptic conditions and treatment was started. S.CRP levels >1mg/dl, total leukocyte count < 5000 cells/cumm, platelets count < 1.5 lakhs/ µL were taken as positive significant (P <0.005) markers for neonatal sepsis. The data was tabulated and subjected to statistical analysis.Results:Positive CRP (>1mg/dl) were found to be highly significant (p<0.0001), Sensitivity, Specificity, PPV, NPV and Diagnostic accuracy were 93.33%,16.00%,76.92%,44.44% and 74.00% respectively. TLC <5000 were found to be significant (p<0.0001), Sensitivity, Specificity, PPV, NPV and Diagnostic accuracy were 65.33%,44.00%,77.78 %,29.73% and 60.00% respectively. Platelet count < 1.5 lakhs/ µL was found to be significant (p<0.0091), Sensitivity, Specificity, PPV, NPV and Diagnostic accuracy were 68.00%, 16.00%,70.83%,14.29% and 55.00% respectively.Conclusions:In developing countries like India, where blood culture investigations are limited, altered haematological parameters such as CRP, TLC, and Platelets counts can serve as quick, simple, economical methods to diagnose neonatal sepsis. Further studies with larger sample size are required to substantiate the results.
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Background:The objective of this study was to assess the demographical characteristic, laboratory and radiological findings associated with COVID-19 mortality in hospitalizedpatients and also to co-relate neutrophil-to-lymphocyte ratio (NLR)and chest x-ray (CXR)score with severity of the disease.Methods:This is a retrospective study done in Bowring and Lady Curzon hospital between the periodof May 2021 to July 2021. 100 patients who were tested positive for SARS-CoV2 with RT-PCR were taken for the study after fulfilling the inclusion criteria. On day 1 of admission, routine blood investigations including CBC with differential count and chestX ray is taken. From the above said data, NLR and CXR score is calculated and a comparison is made to determine severity and in-hospital mortality between mild, moderate and severe COVID pneumonia patients. This study is being carried out after obtaining institutional ethical committee approval clearance. All analysis were performed using SPSS software version 10.Results: The sample size studied was 100. The mean age of patients was 28.3 in mild, 49.9 in moderate and 62.6 in severe COVID patients. Among these 67% were males and 33% were females. It was noted that, leukocytosis(mean-13245), neutrophilia (mean-83.05%), lymphocytopenia (mean-10.45%) and chest X-ray score (mean-4.98) was seen among severe group with p value being significant.Conclusions: TLC, NLR and CXR score were significantly different between severe and non-severe patients, so assessment of these simple parameters may help identify high risk COVID-19 patients at an early stage in a resource limited setting from the data retrieved from our hospital, NLR and CXR Score showed an acceptable efficiency to separate COVID-19 patients among severe and non-severe patients with a significant p value thereby helping in triaging the patients and need for early ICU needs.
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@#Quercetin, a flavonoid compound which is widely distributed in plants are considered ass beneficial physiologically due to attributed bioactivity such as anti-cancer, immunomodulatory, antidiabetic, and anti-inflammatory. In this study, the quercetin content from the dried Blumea balsamifera L. DC dried leaf was macerated with 95% ethanol and the concentrated extract was purified using Modified Kupchan method and flash chromatography. All fractions were tested for the presence of flavonoids using phytochemical screening and the selected dichloromethane fraction were further purified using another round of flash chromatograph. All resulting fractions and pooled samples were tested for the antioxidant property using the developed Thin Layer Chromatography (TLC)-Bioautography and separated compounds were derivatized with DPPH. Using the optimized TLC-Bioautography method, the quercetin content in the dichloromethane fraction was analyzed and compared with a reversed phase high performance liquid chromatography hyphenated with photodiode array detector (RP-HPLC-PDA). The calculated quercetin content from the pooled sample using TLC-bioautography method is 2.25 mg/ml and from RP-HPLC-PDA is 2.02 mg/ml which was not comparable statistically using unpaired t-test (p<0.05, α=0.05
الموضوعات
Quercetinالملخص
Abstract Two sensitive and selective methods were developed for the simultaneous determination of four commonly used non-steroidal anti-inflammatory drugs (NSAIDs), namely; paracetamol (PCM), diclofenac sodium (DCF), ibuprofen (IBP), and indomethacin (IND) in wastewater effluents. The first method used HPLC for the determination of the studied drugs using a mobile phase consisting of phosphate buffer (pH 3.0) and acetonitrile at a flow rate of 1 mL/min. in gradient elution mode and detection at 220 nm. The separation process was performed on BDS Hypersil Cyano column (250 x 4.6 mm, 5 µm). The second method was a TLC-densitometric one which was performed using n-Hexane: ethyl acetate: acetic acid in the ratio (6:3.5:0.5) as a developing system. The proposed chromatographic methods were successfully applied for the selective determination of the four studied drugs in simulated and real pharmaceutical wastewater samples after their solid-phase extraction
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Industrial Effluents , Anti-Inflammatory Agents, Non-Steroidal/analysis , Drug Industry/classification , Wastewater/parasitology , Chromatography, High Pressure Liquid/methods , Acetates/adverse effectsالملخص
Objective To establish the quality standard of Gansu granules (GGs) and effectively control the quality of GGs. Methods TLC identification method of Gansu granules was improved by using pinocembrin-7-O-β-D-glucoside as the indicator. In HPLC analysis, Agilent ZorbaxSB-C18 (4.6 mm×250 mm, 5 μ m) was used as a chromatographic column, and acetonitrile-0.5% formic acid solution was used as the mobile phase. The detection wavelength of 280 nm was used to analyze the content of pinocembrin-7-O-β-D-glucoside in GGs. Results The separation of characteristic spots was good and clear when the established TLC method was used to identify Gansu granules. Quantitative analysis showed that the concentration of pinocembrin-7-O-β-D-glucoside has a good linear relationship with the peak area in the range of 2.4-240 µg/ml (r= 0.9999). The average sample recovery rate of pinocembrin-7-O-β-D-glucoside is 100.76% with RSD value of 0.66%. The accuracy was good. Conclusion The TLC identification method and HPLC content determination method established in this experiment have strong specificity and good reproducibility, and can be used as an improved standard for the quality control of Gansu granules.
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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.
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Objective To revise the qualitative and quantitative determination methods of Xuanxi Rongjin powder. Methods TLC was used to qualitatively identify Chuanxiong and Chuanshanlong. The content of cinnamaldehyde in the preparation was determined by HPLC with KR100-5C18 column (250 mm×4.6 mm, 5μm). The mobile phase was acetonitrile-water (35:65) and the detection wavelength was 290 nm. Results TLC can qualitatively identify Chuanxiong and Chuanshanlong. Cinnamaldehyde has a good linear relationship in the range of 0.0489~0.3260 µg/ml (r=1.00), The average recovery was 95.71% (RSD=1.78%). Conclusion The method has high sensitivity, good specificity, simple operation and good reproducibility.
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ObjectiveTo improve the current standard of Belladonnae Herba in the 2020 edition of Chinese Pharmacopoeia. MethodTaking hyoscyamine sulfate, atropine sulfate and scopoletin as reference substances, and ethyl acetate-methanol-concentrated ammonia(17∶4∶2)as developing solvent, thin layer chromatography (TLC) was applied in the qualitative identification of Belladonnae Herba. The moisture, total ash and ethanol-soluble extract of Belladonnae Herba were determined based on the general principles in the 2020 edition of Chinese Pharmacopoeia (volume Ⅳ). The contents of hyoscyamine sulfate and scopolamine hydrobromide were analyzed by high performance liquid chromatography (HPLC) with mobile phase of acetonitrile-54 mmol·L-1 phosphate buffer solution (14∶86), flow rate of 1.0 mL·min-1 and detection wavelength at 210 nm. ResultThe spots in the TLC were clear with good separation and specificity. Hyoscyamine sulfate and scopolamine hydrobromide showed a good linearity with peak area in the range of 0.024 7-0.789 6 g·L-1 (r=0.999 9) and 0.003 9-0.124 0 g·L-1 (r=0.999 9), the average recoveries of these two ingredients were 100.29% (RSD 1.6%) and 99.04% (RSD 1.4%), respectively. The limits for moisture, total ash in Belladonnae Herba should be less than 13.0% and the limit for the ethanol-soluble extract should be more than 10.0%. Due to the low content and wide variation of scopolamine hydrobromide, the content of hyoscyamine sulfate should not be less than 0.098%. ConclusionThe established method is simple, specific and reproducible, which can be used to improve the quality control standard of Belladonnae Herba.
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ObjectiveTo investigate the quality of Amomi Fructus in the market, and to compare the difference between the seed mass and shell, so as to provide a basis for standardizing the usage of Amomi Fructus. MethodThe properties, thin layer identification, moisture, the content of bornyl acetate were determined by the methods in the 2020 edition of Chinese Pharmacopoeia, and the ash and extract content were determined according to the collection method of the 2020 edition of Chinese Pharmacopoeia. ResultAmong the 17 batches of samples, except the content of bornyl acetate in 2 batches of Amomum longiligulare, 2 batches of A. longiligulare and A. villosum mixture was lower than the standard, the quality of other samples all met the standard of the 2020 edition of Chinese Pharmacopoeia, but there were two specifications with shell and without shell. The husk rate, volatile oil, extract and bornyl acetate contents of the seed mass and shell were tested. It was found that the content of volatile oil in three kinds of Amomi Fructus seed mass was 1.8-5.3 times that of the corresponding shell, and the content of bornyl acetate in the seed mass was 8.8-62.1 times that of the corresponding shell, but there was little difference in the extract content. ConclusionBased on the above research, it is considered that the content of bornyl acetate in A. longiligulare contained in the 2020 edition of Chinese Pharmacopoeia remains to be discussed. It is tentatively determined that the total ash content of Amomi Fructus should not be more than 10.0%, and the extract content should not be less than 15.0%. At the same time, it is suggested that when Amomi Fructus is used as medicine, the dosage of Amomi Fructus should be calculated according to the removal rate of 20%-30% of shell, and it should be crushed regardless of whether it is used in shell or not.
الملخص
ObjectiveTo establish the quality standard of Liangditang benchmark samples. MethodUltra performance liquid chromatography-quadrupole time-of-flight mass spectrometry (UPLC-QTOF-MS) was used to qualitatively analyze the chemical composition of Liangditang on the basis of molecular and fragment ion peak information with cracking law. The mobile phase was methanol (A)-0.05% phosphate aqueous solution (B) for gradient elution (0-10 min, 5%-23.5%A; 10-20 min, 23.5%A; 20-58 min, 23.5%-63%A; 58-60 min, 63%-90%A), the flow rate was 0.8 mL·min-1, and the detection wavelength was 254 nm. Electrospray ionization was employed under positive ion mode, the detection range was m/z 100-1 700. Key quality attributes and sources were determined by comparing with single medicine and reference substances. Through mass transfer analysis of multiple batches from decoction pieces to benchmark samples, high performance liquid chromatography (HPLC) for determining the contents of index components and HPLC detection of characteristic maps were established. Through the determination of 15 batches of benchmark samples, the content range of the index components and the common peaks of the characteristic map were determined. Thin layer chromatography (TLC) was applied to the identification of 5 medicines in the formula. Moisture and dry extract yield of the benchmark samples were determined by drying method. ResultA total of 27 compounds were inferred from the benchmark samples of Liangditang, among which 9 compounds were confirmed by comparison with the control, including catalpol, harpagide, gallic acid, albiflorin, paeoniflorin, verbascoside, angoroside C, cinnamic acid and harpagoside. A method for determining the characteristic maps of the benchmark samples were established and 13 peaks were assigned, and the characteristic peaks were mainly derived from wine-processed products of Rehmanniae Radix, Scrophulariae Radix and wine-processed products of Paeoniae Radix Alba. The similarity between the characteristic map of 15 batches of benchmark samples and the control characteristic map was >0.9. Methods for the determination of paeoniflorin, harpagoside, L-hydroxyproline and glycine were established, and the contents of these four components in 15 batches of benchmark samples were within ±30% of the corresponding mean value, and the transfer rate of decoction pieces to the benchmark samples was stable and controllable. TLC was established to identify 5 prescription drugs (except Ejiao) with two kinds of test solutions, and the results showed that the method had good specificity. The average dry extract yield was 48.06%, and the average moisture was 5.58%, which were within the range of ±10% and ±30% of their mean values, respectively. ConclusionThe quality standard of Liangditang benchmark samples was as follows:the similarity between the benchmark samples and the control characteristic map is >0.9, the contents of paeoniflorin, harpagoside, L-hydroxyproline and glycine are 217-403, 24-46, 634-1 178, 1 253-2 328 mg per dose, the dry extract yield is 43.0%-53.0%, the moisture is 4.0%-7.0%, under the set detection conditions, the benchmark samples have corresponding characteristic spots by comparing with the control herbs of 5 medicines. This quality standard is stable and reliable, which fills the gap in the quality control of Liangditang, and can provide a reference for the establishment of the quality standard of Liangditang granules.
الملخص
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.