Study on Compositional Change of Berchemia lineata from Different Harvest Times

2013 ◽  
Vol 850-851 ◽  
pp. 1267-1270
Author(s):  
Hong Li Teng ◽  
Li Cheng Guo ◽  
Shi Lin Chen
Keyword(s):  
Mobile Phase ◽  
Folk Medicine ◽  
Gradient Elution ◽  
Phosphoric Acid Solution ◽  
Volume Flow ◽  
Elution Volume ◽  
Dynamic Changes ◽  
Column Temperature ◽  
Average Recovery ◽  
Injection Volume

To study content of quercetin in Zhuang folk medicine Berchemia lineata in the different harvest times and to explore the laws of dynamic changes of quercetin content. Methods: determine 10 batches of Berchemia lineata in the HPLC-DAD method. Chromatographic conditions: Agilent XDB C18(150 mm×4.6 mm, 5 μm), the column temperature of 25 °C; mobile phase of methanol (A) - acetonitrile (B) -0.05% phosphoric acid solution (C), gradient elution; volume flow of 1 mL/min, detection wavelength of 254 nm. Result: sample injection volume of quercetin in the range of 0.69 μg ~ 4.83 μg has a good linear relationship with peak area, the average recovery is 99.8%, RSD: 1.27% (n = 6). From the overall analysis, content of quercetin in Berchemia lineata harvested in January is higher than that in other months. Conclusion: January should be the best month for harvest of Berchemia lineata.

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 Simultaneous and Trace Level Determination of Six Potential Impurities by UPLC-ESI-MS/MS in Antiarrhythmic Drug: Dronedarone Hydrochloride

2020 ◽  
Vol 32 (5) ◽  
pp. 1183-1190
Author(s):  
K. Durga Raja ◽  
V. Saradhi Venkata Ramana ◽  
K. Raghu Babu ◽  
B. Kishore Babu ◽  
V. Jagadeesh Kumar ◽  
...  
Keyword(s):  
Mobile Phase ◽  
Gradient Elution ◽  
Ultra Performance Liquid Chromatography ◽  
Solvent Mixture ◽  
Column Temperature ◽  
Esi Ms ◽  
Quantitation Limit ◽  
Ich Guidelines ◽  
Validation Tests ◽  
Development And Validation

Development and validation of six potential impurities by ultra performance liquid chromatography electro spray ionization tandem mass (UPLC-ESI-MS/MS) method for dronedarone hydrochloride drug was accomplished coherent with ICH guidelines. Successful chromatographic separation of dronedarone with its six impurities was attained by using gradient elution mode on RP-UPLC column using three pump mode system of 0.1 % formic acid in water as mobile phase A, methanol as the mobile phase B and solvent mixture of methanol, acetonitrile and water in the ratio of 65:30:5 v/v/v as the mobile phase C. Chromatographic conditions were set as 0.3 mL min-1 flow rate at the column temperature of 45 °C with the injection volume 2 μL. Briefly, the method enabled quantitation of six impurities with high accuracy (recovery > 90 %) and precision (% RSD < 5.0),within the ranges of 0.18-2.82 μg g-1. The regression (r) for each impurity over a range was > 0.99. The detection limit and quantitation limit of impurities were set at 0.09 and 0.18 μg g-1, respectively. The performed validation tests proved the suitability of the method for its intended purposes.

scholarly journals DETERMINATION OF 2-CYANO-4’-BROMOMETHYL BIPHENYL GENOTOXIC IMPURITY IN IRBESARTAN DRUG SUBSTANCES USING HPLC TECHNIQUE

2016 ◽  
Vol 8 (12) ◽  
pp. 225
Author(s):  
S. Senthil Kumar ◽  
Ritesh Kumar Srivastava ◽  
V. Srinivas Rao
Keyword(s):  
Mobile Phase ◽  
Hplc Method ◽  
Development Activity ◽  
Validation Data ◽  
Column Temperature ◽  
Injection Volume ◽  
Drug Substances ◽  
Hplc Technique ◽  
Ich Guideline

<p><strong>Objective: </strong>The objective of present study was to develop and validate a specific and sensitive HPLC method for the quantitative determination of genotoxic impurity 2-cyano-4’-bromomethyl biphenyl present in irbesartan drug substance.</p><p><strong>Methods: </strong>The development activity was conducted by HPLC with UV as a detector. The impurity was separated on Kromasil C18 250 x 4.6 mm, 5 µm analytical column with a mobile phase consisting of buffer pH 3.2 and acetonitrile in the ratio of 60:40 v/v at a flow rate 1.5 ml/min. The effluent was monitored by UV detection at 258 nm with column temperature maintained at 40 °C and the injection volume 30 μl. Acetonitrile was selected as diluent.</p><p><strong>Results: </strong>Validation activity was planned and completed based on the ICH guideline. The LOD and LOQ value were found to be 0.167 µg/g and 0.506 µg/g and accuracy results were well in the range 98.34 to 103.46 %. The linearity curve showed the correlation coefficient of 0.9999 and method very sensitive.</p><p><strong>Conclusion: </strong>From validation data, it was confirmed that the developed method is specific, sensitive, linear, precise and accurate for the determination of 2-cyano-4’-bromomethyl biphenyl genotoxic impurity in irbesartan drug substances.</p>

scholarly journals Study on chemical constituents of different species of Dendrobium

2020 ◽  
Vol 165 ◽  
pp. 05026
Author(s):  
Zhenghui Wan ◽  
Qingjun Huang
Keyword(s):  
Mobile Phase ◽  
Research Method ◽  
High Performance ◽  
Chemical Constituents ◽  
Chromatographic Peak ◽  
Column Temperature ◽  
Injection Volume ◽  
Chinese Pharmacopoeia ◽  
Processing Techniques ◽  
Theoretical Plates

The objective of this study is to determine the erianin of 10 species of Dendrobium by high performance liquid chromatography (HPLC). Processing techniques were washed, dried and ground. The research method for determining the content of erianin was adopted from Chinese Pharmacopoeia 2015 Edition. Acetonitrile-0.05% phosphoric acid (37:63) was used as mobile phase. The samples were separated on Sharpsil-TC18 column(4.6*150mm;5μm) at a flow rate of 1.2mL/min and detected at 230nm, and the column temperature was kept at 30℃. The injection volume was 20μL. The number of theoretical plates was not less than 6000 according to the chromatographic peak of erianin. The result of the study showed erianin was detected only in Dendrobium chrysotoxum among the 10 species of Dendrobium. and the content was 0.098%. Conclusion: The content of erianin in Dendrobium chrysotoxum met the specification of no less than 0.03% in the 2015 edition of Chinese Pharmacopoeia.

Gradient Elution Separation of Main Ingredients from Polygoni Multiflori Extract by HPLC

2013 ◽  
Vol 864-867 ◽  
pp. 503-507
Author(s):  
Tao Wang
Keyword(s):  
Gradient Method ◽  
Mobile Phase ◽  
Separation Efficiency ◽  
Gradient Elution ◽  
Polygonum Multiflorum ◽  
Uv Detector ◽  
Experimental Conditions ◽  
Column Temperature ◽  
Stilbene Glucoside

In this experiment, the main compounds of stilbene glucoside and anthraquinones from polygonum multiflorum extract were separated by HPLC gradient elution. SinoChrom ODS-BP C18 is selected as chromatographic column. The optimal experimental conditions under 254nm wavelength UV detector include the column temperature: 26°C, mobile phase: methanol/water, and flow rate: 1.0ml/mol. The gradient method can be optimized by changing the steepness and shape of gradient elution. Through optimizing gradient method, the separation efficiency is improved within a certain range of gradient elution strength. This article provides important reference for quality control and content determination of fleece-flower root.

Determination of Genotoxic alkyl p-toluene Sulfonates in Cabazitaxel using LC-MS Method

2019 ◽  
Vol 15 (7) ◽  
pp. 753-761
Author(s):  
Bavireddi Mohan ◽  
Ramayanam Siva Kameswara Sharma ◽  
Devarakonda Ravi Kumar ◽  
Seshagiri Vijaya Murali Mohan Rao ◽  
Nutulapati Venkata Satya Venugopal
Keyword(s):  
Mobile Phase ◽  
Ammonium Acetate ◽  
Dosage Forms ◽  
Column Temperature ◽  
Ammonium Acetate Buffer ◽  
Injection Volume ◽  
Ich Guidelines ◽  
Genotoxic Impurities ◽  
Pharmaceutical Laboratories

Introduction: A suitable LC-MS method for the quantitative determination of genotoxic impurities such as alkyl p-toluene sulfonates in Cabazitaxel was developed. Alkyl p-toluene sulfonates were estimated by LC-MS method using Waters Symmetry C18 (75×4.6 mm), 3.5 µ column. Materials and Methods: Column temperature was maintained 40 °C. Injection volume was 10 µL and flow rate was set as 0.8 mL/min. Sampler temperature was maintained to 25 °C and run time was set as 25 minutes. The mobile phase was a mixture of ammonium acetate buffer and acetonitrile in 70:30(v/v) was used. Results: The method validation has been carried as per ICH guidelines. LOQ was found to be 2.66 µg/mL, 2.75 µg/mL and 2.55 µg/mL for MPTS, EPTS and IPPTS Alkyl p-Toluene Sulfonates (APTS) respectively. Conclusion: The proposed Liquid chromatography-Mass spectroscopy method that can quantify genotoxic APTS in Cabazitaxel at low-level concentration has been developed and validated as per ICH guidelines. Hence, the proposed method was recommended for the assay of genotoxic impurities of cabazitaxel in dosage forms in busy pharmaceutical laboratories.

UPLC-ESI-MS/MS Method for Determination of Recombinant Antihypertensive Peptide in Rat Plasma

2015 ◽  
Vol 730 ◽  
pp. 254-259 ◽  
Author(s):  
Yan Li Cong ◽  
Shen Li ◽  
Bo Chen ◽  
Hai Yan Sun ◽  
Dong Liu ◽  
...  
Keyword(s):  
Mass Spectrometry ◽  
Mobile Phase ◽  
Gradient Elution ◽  
Rat Plasma ◽  
Plasma Samples ◽  
Selected Ion Monitoring ◽  
Column Temperature ◽  
Qualitative And Quantitative ◽  
Esi Ms

The focus of the study was to establish an UPLC-ESI-MS/MS method for the qualitative and quantitative determination of VLPVPR in rat plasma. The method was as follows: Protein impurities in the rat plasma samples were precipitated with methanol; A Waters Acquity BEH C18 column (100 mm×2.1 mm, 1.7 μm) was adopted; the column temperature was 25°C; the mobile phase consisted of methanol-water with gradient elution at the steady flow rate of 0.3 mL·min-1; the detection wavelength was 202 nm. Mass spectrometry applied selected ion monitoring mode with m/z 255 (quantitative ion) and m/z 169 (qualitative ion). It was found that excellent linear relationship was obtained from the range of 10~200 ng·mL-1 (r=0.9991), the limit determination (LOD) of VLPVPR was 1.8 ng·mL-1, the recovery rate was 96.33%~100.76%, The inter and intre-day RSD were less than 7%. We thus conclude that a rapid and sensitive UPLC-ESI-MS/MS method was developed and validated for the determination of recombinant antihypertensive peptide VLPVPR in rat plasma. It can be applied to evaluate the pharmacokinetics of VLPVPR.

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.

Establishment and Evaluation of Determination of Cinnamaldehyde in Baoyuanqingxue Granules by HPLC

2014 ◽  
Vol 998-999 ◽  
pp. 372-377 ◽  
Author(s):  
Qiang Wu ◽  
Chang Hong Wang ◽  
Pu Wang ◽  
Xiang Rong Liu
Keyword(s):  
Quality Control ◽  
High Performance Liquid Chromatography ◽  
Liquid Chromatography ◽  
Extraction Method ◽  
Mobile Phase ◽  
High Performance ◽  
Hplc Method ◽  
Column Temperature ◽  
Average Recovery

To examine the extraction method and chromatographic conditions that affect the determination of cinnamaldehyde in Baoyuanqingxue granules and make clinical evaluation about the determination of cinnamaldehyde.Ultrasonic methanol extraction was used before the detemination of cinnamaldehyde in Baoyuanqingxue granules. High Performance Liquid chromatography (HPLC) method was applied to detect samples. The SB-C18 column (Agilent, ZORBAX, 4.6×150mm, 5μm) was adopted, the mobile phase was acetonitrile-water (35:65) at the flow rate of 1.00mL•min-1 with DAD detection wavelength at 290nm, the volume of injection was 20μL and the column temperature was 30°C. The resolution between cinnamaldehyde and other peaks was good. The calibration curve was linear in the range of 0.5035~50.35μg•mL-1(r=0.99976). The average recovery (n=6) of cinnamaldehyde was 99.2% with RSD of 0.5%. The HPLC-DAD method to detect the content of cinnamaldehyde in Baoyuanqingxue granules is simple and accurate. It can be used for quality control of cinnamaldehyde in Baoyuanqingxue granules.

Quantitative Determination of Anthraquinones and Resveratrol in Polygonum Cillinerve (Nakai) Ohwi by HPLC-PAD

2017 ◽  
Vol 100 (1) ◽  
pp. 25-29 ◽  
Author(s):  
Yanfang Wu ◽  
Xinsheng Wang ◽  
Pu Liu ◽  
Qingshan Niu ◽  
Qinan Wu
Keyword(s):  
Mobile Phase ◽  
High Performance ◽  
Geographical Area ◽  
Gradient Elution ◽  
Reversed Phase ◽  
Column Temperature ◽  
Photodiode Array ◽  
Funiu Mountain ◽  
Phase Column

Abstract A simple, sensitive, and validated high-performance liquid chromatography-photodiode array method has been established for the simultaneous determination of anthraquinones and resveratrol in Polygonum Cillinerve (Nakai) Ohwi (Zhushaqi in Chinese). The evaluation was performed using a Sunfire C18 reversed-phase column with 30°C column temperature. The mobile phase was composed of a gradient elution of 0.5% acetic acid (solvent A) and methanol (solvent B) with flow rate of 1.0 mL/min. The detection wavelength was at 254nm. The method developed and validated is simple, shows good linearity, sensitivity, precision, and recovery, and is applied to analyze anthraquinones and resveratrol in 13 batches of Zhushaqi. The results show that the target compounds of Zhushaqi are significantly different among these samples. Based on results of the statistical analysis, the samples collected from Funiu Mountain were clustered together, and the samples obtained fromBozhou Market were close together. The developed method can be a useful tool in quality control and used to evaluate difference and to identify the geographical area of Zhushaqi, and also to provide technical support for the pharmacological and clinical research of related drugs.

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