scholarly journals Establishment of the Quantitative Analysis of Multiindex in Euphorbia lathyris by the Single Marker Method for Euphorbia lathyris Based on the Quality by Design Concept

2021 ◽  
Vol 2021 ◽  
pp. 1-8
Author(s):  
Feng Xuehua ◽  
Zhou Guangjiao ◽  
Tao Ali
Keyword(s):  
Flow Rate ◽  
Standard Method ◽  
Mobile Phase ◽  
Column Temperature ◽  
Injection Volume ◽  
External Standard Method ◽  
Relative Standard ◽  
Significant Difference ◽  
External Standard ◽  
Euphorbia Lathyris

Methods. The influences of methanol proportion, flow rate, column temperature, and injection volume in the mobile phase on the chromatographic resolution of chromatographic peak of euphorbia factor L1 were experimentally studied via Plackett–Burman design, and the key analysis parameters were screened out; the key analysis parameters were optimized through the central composite design, and the chromatographic analysis conditions were established. Euphorbia factor L1 was taken as the internal reference to construct the relative correction factors for L3 and L4 relative to L1, and their contents were calculated, thus realizing the QAMS. Meanwhile, the euphorbia factor L3 and euphorbia factor L4 were determined using the external standard method, and the differences of values measured by the external standard method from the values predicted by the QAMS method were compared, in an effort to verify the accuracy and feasibility of the QAMS method. Results. The methanol proportion and column temperature in the mobile phase were the key analysis parameters P < 0.05 , and the chromatographic conditions were determined as follows. The methanol/water ratio, column temperature, detection wavelength, flow rate, and injection volume were 60 : 40, 30°C, 275 nm, 1.0 mL/min, and 10 μL, respectively. A total of 20 batches of samples were determined by the QAMS method and external standard method; the relative standard deviations (RSDs) of L3 and L4 determination results were less than 2.0%, without any significant difference. Conclusion. The QbD-based QAMS method can be used to determine the contents of euphorbia factor L3 and euphorbia factor L4 in Euphorbia lathyris L., and it is accurate and feasible.

Detection of 9α-OH-AD Prepared by Biotransformation

2013 ◽  
Vol 821-822 ◽  
pp. 1005-1008
Author(s):  
Li Min Ma ◽  
Li Cui ◽  
Yu Hang Zhao
Keyword(s):  
Quality Control ◽  
Correlation Coefficient ◽  
Flow Rate ◽  
Standard Method ◽  
Mobile Phase ◽  
Average Recovery ◽  
Rp Hplc ◽  
External Standard Method ◽  
External Standard

Detection of 9а-OH-AD prepared by biotransformation by RP-HPLC directly was studied.The detection is performed on a Kromasil 100-5C18(4.6×250mm) column, using methanol:water(7:3,v/v)as mobile phase,0.8mL•min-1flow rate and external standard method,deteced at 242nm.There is a good line correlaction between peak and content in range of 0.01-0.20g/L,the correlation coefficient is 0.9942,the average recovery is 99.09% with a relative stand deviation of 0.89%(n=5).The method is simple,stable,accurate and reliable for quality control of 9а-OH-AD.

Determination of Paeoniflorin and Paeonol in Houyinan Tablet by UPLC

2012 ◽  
Vol 581-582 ◽  
pp. 68-72
Author(s):  
Chu Qin Yu ◽  
Hua Qing Lin ◽  
Yue Han Hou ◽  
Zhong Feng Shi ◽  
Di Shi Lin
Keyword(s):  
Quality Control ◽  
Simultaneous Determination ◽  
Flow Rate ◽  
Mobile Phase ◽  
Gradient Elution ◽  
The Other ◽  
Column Temperature ◽  
Average Recovery ◽  
Injection Volume

In this study, our purpose was to establish a UPLC method for the simultaneous determination of Paeoniflorin and Paeonol in Houyinan Tablet. The separation was performed on Acquity BEH C18 column(2.1mm×100mm,1.7μm), the mobile phase was acetonitrile-water with gradient elution at a flow rate of 0.2 mL•min-1, the detection wavelength was 230nm, the column temperature was 30°Cand the injection volume was 2μL. Paeoniflorin and Paeonol reached effective separation with the other components in this chromatographic conditions. Paeoniflorin and Paeonol were linear within the range of 0.0406~0.4064μg(r=0.9999) and 0.0426~0.4256μg (r=0.9999), respectively. The average recovery was 99.82% and 100.6%. The results of method validation indicated that the method was simple,quick,accurate, specific and less solvent consumption. It can be used for the quality control of Houyinan Tablet.

scholarly journals DEVELOPMENT AND VALIDATION OF A FAST AND SENSITIVE UHPLC-PDA METHOD FOR THE QUANTIFICATION OF URSOLIC ACID IN POLY(L-LACTIC ACID) NANOCAPSULES

2020 ◽  
pp. 161-165
Author(s):  
BRUNA CARLETTO ◽  
AMANDA MARTINEZ LYRA ◽  
ADRIANA YURIKO KOGA ◽  
ANDRESSA NOVATSKI ◽  
RUBIANA MARA MAINARDES ◽  
...  
Keyword(s):  
Lactic Acid ◽  
Ursolic Acid ◽  
Flow Rate ◽  
Mobile Phase ◽  
High Performance ◽  
Limits Of Detection ◽  
Column Temperature ◽  
Relative Standard ◽  
Development And Validation ◽  
Detection And Quantification

Objective: The aim of the present study is to develop and validation of a ultra-high performance liquid chromatography (UHPLC) method to determine the ursolic acid content and its encapsulation efficiency (EE) in lipid-core nanocapsules prepared from poly (L-lactic acid). Methods: A simple UHPLC-PDA method was developed and validated for the quantitative determination of ursolic acid in poly(L-lactic acid) nanocapsules. The chromatographic conditions used were: RP-C18 column, isocratic mobile phase containing acetonitrile:water (92:8, v/v), flow rate of 0.8 ml/min, column temperature of 50°C, and detection at 203 nm. The following parameters were evaluated: Specificity, linearity, limits of detection and quantification, precision, accuracy, and robustness. Results: The method was specific to the ursolic acid and linear (r=0.9998) in the range of 10–100 μg/ml. The limits of detection and quantification were 1.35 and 4.10 μg/ml, respectively. The precision was demonstrated by a relative standard deviation less than 2%. Adequate accuracy (98.35%±0.82) was obtained. Changes in flow rate, mobile phase, and column temperature did not significantly alter the peak area and the retention time of the ursolic acid. The mean EE was 99.89%. Conclusion: The method proved to be fast, sensitive, and simple for quantifying ursolic acid in nanocapsules and was successfully used for determining the EE.

Determination of Patulin Residues in Canned Fruits by HPLC

2014 ◽  
Vol 1004-1005 ◽  
pp. 936-940
Author(s):  
Ling Lin ◽  
Chun Liang Yang ◽  
Shao Dong Zeng ◽  
Qi Li ◽  
Hong Bin Guo
Keyword(s):  
Standard Method ◽  
Mobile Phase ◽  
Limit Of Detection ◽  
Constant Volume ◽  
Uv Detection ◽  
External Standard Method ◽  
Fruit Samples ◽  
External Standard ◽  
Sensitive Method

A sensitive method for determining residues of patulin in canned fruits was established by HPLC.Canned fruit samples were extracted with acetonitrile and purified through multifunctional cleanup column.Collected purifying liquids and blowed N2 to nearly dry,and then using the mobile phase to dissolve and constant volume, and were determined by UV detection at 276 nm with external standard method for quantitative, the recovery rates of patulin in canned fruits were 80%~95%, The RSD were of 2.2%~6.5%,the limit of detection was 0.012 μg /kg for patulin.

Liquid Chromatographic Assay of Bentazon Formulations

1993 ◽  
Vol 76 (2) ◽  
pp. 387-389
Author(s):  
Thomas M Schmitt
Keyword(s):  
Standard Method ◽  
Mobile Phase ◽  
Chromatographic Method ◽  
Active Agent ◽  
Reversed Phase ◽  
External Standard Method ◽  
Liquid Chromatographic Method ◽  
External Standard ◽  
Phase Liquid ◽  
Liquid Chromatographic

Abstract A reversed-phase liquid chromatographic method is presented for determining the active agent in technical bentazon and in aqueous formulations of the sodium salt of bentazon. The procedure is an isocratic, external standard method specifying an octadecylsilyl column, an acetate-buffered mobile phase of methanol-water, and UV detection. The 340 nm detection wavelength eliminates interference from formulation impurities.

scholarly journals Analysis of the HPLC Fingerprint and QAMS for Sanhuang Gypsum Soup

2018 ◽  
Vol 2018 ◽  
pp. 1-14 ◽  
Author(s):  
Yi Peng ◽  
Minghui Dong ◽  
Jing Zou ◽  
Zhihui Liu
Keyword(s):  
Quantitative Analysis ◽  
Standard Method ◽  
Evaluation Method ◽  
Similarity Analysis ◽  
Hplc Fingerprint ◽  
External Standard Method ◽  
Significant Difference ◽  
External Standard ◽  
Single Marker

A valid and encyclopaedic evaluation method for assessing the quality of Sanhuang Gypsum Soup (SGS) has been set up based on analysis of high-performance liquid chromatography (HPLC) fingerprint combined with the quantitative analysis of multicomponents by single marker (QAMS) method, hierarchical cluster analysis (HCA), and similarity analysis. 20 peaks of the common model were obtained and used for the similarity analysis and HCA analysis. Berberine was selected as an internal reference, and the relative correction factors of mangiferin, geniposide, liquiritin, epiberberine, coptisine, baicalin, palmatine, harpagosid, wogonoside, cinnamic acid, cinnamic aldehyde, baicalein, glycyrrhizic acid, and wogonin were established. The accuracy of quantitative analysis of multicomponents by the single-marker method was verified by comparing the contents of the fourteen components calculated by the external standard method with those of the quantitative analysis of multicomponents by the single-marker method. No significant difference was found in the quantitative results of the established quantitative analysis of multicomponents by a single-marker method and an external standard method. In summary, these methods were applied to evaluate the quality of SGS successfully. As a result, these evaluation methods have great potential to be widely used in the quality control of traditional Chinese medicines (TCM).

scholarly journals Simultaneous Determination of Six Active Components in Oviductus Ranae via Quantitative Analysis of Multicomponents by Single Marker

2017 ◽  
Vol 2017 ◽  
pp. 1-9 ◽  
Author(s):  
Shihan Wang ◽  
Yang Xu ◽  
Yanwei Wang ◽  
Huailei Yang ◽  
Zuying Lv ◽  
...  
Keyword(s):  
Quantitative Analysis ◽  
Standard Method ◽  
Internal Standard ◽  
Active Components ◽  
External Standard Method ◽  
Significant Difference ◽  
External Standard ◽  
Single Marker ◽  
Quantitative Results ◽  
Oviductus Ranae

A method, quantitative analysis of multicomponents by single marker (QAMS), was established in this article to investigate the quality control of a traditional Chinese medicine, Oviductus Ranae. 7-Hydroxycholesterol, 7-ketocholesterol, 4-cholesten-3-one, stigmasterol, 7-dehydrocholesterol, and cholesterol were selected as the indexes of quality evaluation of Oviductus Rana. The determination was achieved on an Agilent HC-C18 column (4.6 mm × 250 mm, 5 μm) using methanol with water (87 : 13 v/v) as mobile phase at the flow rate of 2.0 mL/min. Cholesterol was used as an internal standard to determine the relative correction factors between cholesterol and other steroidal constituents in Oviductus Ranae. The contents of those steroidal constituents were calculated at the same time. To evaluate the QAMS method, an external standard method was used to determine the contents of six steroidal constituents. No significant difference was observed when comparing the quantitative results of QAMS with the results of external standard method. The proposed QAMS method was proved to be accurate and feasible based on methodological experiments. QAMS provided a simple, efficient, economical, and accurate way to control the quality of Oviductus Ranae.

scholarly journals Stability indicating HPLC-Fluorescence detection method for the simultaneous determination of linagliptin and empagliflozin in their combined pharmaceutical preparation

2021 ◽  
Vol 12 (2) ◽  
pp. 168-178
Author(s):  
Mohamed Rizk ◽  
Ali Kamal Attia ◽  
Heba Yosry Mohamed ◽  
Mona Elshahed
Keyword(s):  
Fluorescence Detection ◽  
Mobile Phase ◽  
Pharmaceutical Preparation ◽  
Pharmaceutical Preparations ◽  
Forced Degradation ◽  
Stability Indicating ◽  
Accuracy And Precision ◽  
Relative Standard ◽  
Significant Difference

A sensitive, accurate, and precise liquid chromatographic method has been developed and validated for the determination of Linagliptin (LNG) and Empagliflozin (EMP) in their combined tablets. Chromatographic separation was carried out on ODS-3 Inertsil® C18 column (150×4.6 mm, 5 µm). The mobile phase A (consisting of 0.30% Triethyl amine buffer (TEA) at pH = 4.5, adjusted using ortho-phosphoric acid); the mobile phase B (consisting of acetonitrile) was pumped through the column whose temperature was maintained at 40 °C, with a flow rate 1.7 mL/min, using gradient elution from 0-3 min A:B (75:25, v:v), then from 3-6 min the ratio changed to be A:B (60:40, v:v). Fluorescence detection (FLD) was performed at 410 nm after excitation at 239 nm. Acceptable linearity, accuracy and precision values of the proposed method were found over the concentration ranges of 0.5-15 µg/mL for LNG and 1.0-30 µg/mL for EMP with correlation coefficients of 0.9997 and 0.9998 in the case of LNG and EMP, respectively. The recoveries and relative standard deviations percentages were found in the following ranges: 98.56-101.85 and 0.53-1.52% for LNG and 98.00-101.95 and 0.31-1.05% for EMP. The detection and quantification limits were 0.15 and 0.45 µg/mL for LNG and 0.22 and 0.67 µg/mL for EMP. The optimized method was validated and proved to be specific, robust, accurate and reliable for the determination of the drugs in pure form or in their combined pharmaceutical preparations. No significant difference was found regarding accuracy and precision upon statistical comparison between the obtained results of the proposed method and those of the reported method. Furthermore, the proposed method is proved to be a stability-indicating assay after exposure of the studied drugs to variable forced degradation parameters, such as acidic, alkaline and oxidative conditions, according to the recommendations of the International Conference on Harmonization guidelines. The simplicity and selectivity of the proposed method allows its use in quality control laboratories.

scholarly journals A New Validated Stability Indicating RP-HPLC Method for Simultaneous Quantification of Formoterol Fumarate Dihydrate and Mometasone Furoate in Metered Dose Inhalation Aerosol

2021 ◽  
Vol 33 (11) ◽  
pp. 2723-2728
Author(s):  
Surya Prakash Mamillapalli ◽  
Gourabattina Lakshmi Prasanna ◽  
B. Venkata Subbaiah ◽  
N. Annapurna
Keyword(s):  
Flow Rate ◽  
Mobile Phase ◽  
Hplc Method ◽  
Mometasone Furoate ◽  
Simultaneous Estimation ◽  
Column Temperature ◽  
Stability Indicating ◽  
Metered Dose ◽  
Formoterol Fumarate ◽  
Dose Inhalation

Stability indicating reversed phase-HPLC method for simultaneous estimation of mometasone furoate (MAF) and formoterol fumarate (FFD) in metered dose inhalation aerosol (MDI) dosage formulation has been developed and discussed in the present work. The chromatographic separation was achieved using Hypersil ODS column (250 mm × 4.6 mm, 3 μm) using an isocratic separation mode at a flow rate of 1.2 mL/min, column temperature of 50 ºC. The system operates with a mobile phase comprising of solution-A (buffer): Solution-B (acetonitrile) mixed in the ratio of 70:30 %v/v at a UV detection wavelength of 214 nm. Retention times of mometasone furoate and formoterol fumarate found to be about 3 min and 7 min, respectively. All possible degradation products of both compounds were monitored at 214 nm and spectral purity along with % mass balance is assessed using PDA detector. Both analyte were subjected to force degradation studies, found all degradants were resolved from analyte peaks and also other process-related impurities. The proposed method is validated for specificity, linearity, accuracy, precision and robustness as per ICH guidelines and found to be adequate. Method stood to be robust with variation in column temperature, flow rate, pH of buffer and organic content in mobile phase.

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