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.

Detection, Quantitation, and Identification of Residual Aminopenicillins by High-Performance Liquid Chromatography after Fluorescamine Derivation

2000 ◽  
Vol 63 (10) ◽  
pp. 1421-1425 ◽  
Author(s):  
CHIH-CHUN HONG ◽  
FUSAO KONDO
Keyword(s):  
Bovine Serum ◽  
Mobile Phase ◽  
High Performance ◽  
Serum Proteins ◽  
Limit Of Detection ◽  
Solid Phase ◽  
Excitation Wavelength ◽  
Column Temperature ◽  
Solid Phase Extraction Cartridge ◽  
Mobile Phases

A high-performance liquid chromatographic (HPLC) method with fluorescence detection after precolumn fluorescamine derivation was developed to detect residues of two aminopenicillins, amoxicillin (AMPC) and ampicillin (ABPC), in bovine serum. Proteins in serum samples spiked with each of these penicillins were precipitated with sodium tungstate and sulfuric acid, centrifuged, and removed by passage through a C18 solid-phase extraction cartridge. After precolumn treatment of the extraction products of AMPC and ABPC with fluorescamine solution, HPLC analysis with fluorescence spectrophotometric detection at an excitation wavelength of 390 nm and an emission wavelength of 485 nm was performed to identify these products. Two mobile phases were used for residual analysis by the isocratic HPLC system. An ODP column (polyvinyl alcohol bonded with an octadecyl functional group) that can be used with strongly alkaline mobile phases (pH 2.0 to 13) was selected, and the column temperature was set at 40°C. A mobile phase comprising 100-mM K2HPO4 solution and acetonitrile (72:28, vol/vol), which yielded AMPC and ABPC retention times of 4.1 and 7.9 min, respectively, was suitable for detection of residual ABPC but not for residual AMPC because interference was caused by peaks of other extracted substances. When a mobile phase comprising a different ratio of 100-mM K2HPO4 solution and acetonitrile (78:22, vol/vol) was used, the retention times of AMPC and ABPC were 7.3 and 26.3 min, respectively, and both penicillins could be analyzed using this system. The calculated standard curves of the reaction products with both mobile phases were linear, and the correlation coefficients were greater than 0.999. The lower limit of detection was 10 ng/ml for both penicillins. Analysis of extracts from bovine serum spiked with AMPC and ABPC at a concentration of 1 μg/ml yielded recovery rates of 102.2 ± 5.5% and 79.0 ± 5.2%, respectively. This detection method may be useful for routine laboratory testing of AMPC and ABPC.

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 Thermodynamic and Extrathermodynamic Studies of Enantioseparation of Imidazolinone Herbicides on Chiralcel OJ Column

2013 ◽  
Vol 2013 ◽  
pp. 1-9 ◽  
Author(s):  
Wenjian Lao
Keyword(s):  
High Performance Liquid Chromatography ◽  
Chiral Separation ◽  
Mobile Phase ◽  
High Performance ◽  
Chromatographic Peak ◽  
Chiral Column ◽  
Higher Temperature ◽  
Lower Temperature ◽  
The Moment ◽  
Imidazolinone Herbicides

A homologous series of chiral imidazolinone herbicide was previously resolved on Chiralcel OJ column in high performance liquid chromatography. However, the mechanism of the chiral separation remains unclear. In this study, chromatographic behaviors of five chiral imidazolinone herbicides were characterized by thermodynamic and extrathermodynamic methods in order to enhance the understanding of the chiral separation. Thermodynamic parameters of this study were derived from equilibrium constant () that was estimated from the moment analysis of the chromatographic peak. Van't Hoff plots of ( versus ) were linear at a range of 15–50°C, only nonlinear at a range of 5–15 °C with n-hexane (0.1%, trifluoroacetic acid)-2-propanol 60/40 (v/v) mobile phase. The enantiomer retention on the chiral column was entropy-driven at a lower temperature (5°C) and enthalpy-driven at a higher temperature (10 to 50°C). Enantioseparations of four of the five imidazolinone herbicides were enthalpy-driven, only entropy-driven for imazaquin. Enantioseparation mechanisms were different in between 5–10°C and 15–50°C probably due to the conformational change of the OJ phase. Enthalpy-entropy compensation showed similar mechanisms in retention and chiral separation for the five or enantiomers. Several extrathermodynamic relationships were able to be extracted to address additivity of group contribution.

scholarly journals THE OPTIMIZATION OF HPLC FOR QUANTITATIVE ANALYSIS OF ACID ORANGE 7 AND SUDAN II IN COSMETIC PRODUCTS USING BOX BEHNKEN DESIGN

2019 ◽  
pp. 130-137 ◽  
Author(s):  
NOVALINA BR PURBA ◽  
ABDUL ROHMAN ◽  
SUDIBYO MARTONO
Keyword(s):  
Flow Rate ◽  
Retention Time ◽  
Mobile Phase ◽  
High Performance ◽  
Hplc Method ◽  
Acid Orange 7 ◽  
Column Temperature ◽  
Box Behnken Design ◽  
Acid Orange

Objective: The objective of this study was to optimize high-performance liquid chromatography (HPLC) method for the determination of acid orange 7 (AO7) and sudan II (SII) in blusher product based on response surface methodology using box behnken design (BBD) approach. Methods: Some factors responsible for HPLC separation including column temperature, mobile phase composition, flow rate were optimized using BBD. The responses evaluated were peak area, retention time, and tailing factor. AO7 and SII in blusher product has different properties, therefore both analytes were analysed using C18 column (Thermo Synergy Gold 250 mm x 4.6 mm i.d.,5 µm) using Shimadzu LC 20AD chromatograph equipped with photo-diode array (PDA) detector at 300-650 nm. The mobile phase used was acetonitrile-water (1:1 v/v), and acetonitrile composition was optimized at 35-50% for separation AO7 (ACN1), and 80-90% for SII (ACN2), delivered at the flow rate of 0.9–1 ml/min, using column temperature at 30-40 °C. Results: BBD showed that separation of AO7 was influenced by the concentration of ACN1, flow rate and column temperature. These factors affected retention time, peak area, and tailing factor with peak area was the most significant. Tailing factor was not significantly affected by each factor, and retention time was slightly effected. Otherwise, Sudan II was affected by all these factors except ACN1. The optimal condition obtained based BBD was ACN1 43%, ACN2 90%, the flow rate of 0.9 ml/min and a column temperature of 40 °C. Conclusion: BBD can be used to get optimum condition for analysis of AO7 and SII in blusher product.

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.

Analysis of Bifenthrin and its Enantiomer Using High Performance Liquid Chromatography

2014 ◽  
Vol 675-677 ◽  
pp. 275-279 ◽  
Author(s):  
Su Su Fan ◽  
Jian Shi ◽  
Ling Zhou ◽  
Yu Wen Hang
Keyword(s):  
High Performance Liquid Chromatography ◽  
Liquid Chromatography ◽  
Mobile Phase ◽  
High Performance ◽  
Chiral Stationary Phase ◽  
Ammonium Acetate ◽  
Hplc Method ◽  
Column Temperature ◽  
Polysaccharide Derivatives ◽  
Separation Results

Using the high performance liquid chromatography (HPLC) method, bifenthrin isomers can be split at a polysaccharide derivatives chiral stationary phase column, and two well distinguished peaks of bifenthrin isomers are obtained. The effects of mobile phase ratios, temperatures, and detection wavelengths on the separation results are discussed. The optimal chromatographic conditions are as follows: the mobile phase ratio is methanol: ammonium acetate salts = 80:20, the column temperature is 35°C, and the wavelength is set as 220 nm. Under the optimal conditions, the resolution of bifenthrin enantiomer can be as large as 3.0.

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.

scholarly journals Related Impurities High-performance Liquid Chromatography Method Development and Validation for drug combinations: Olmesartan Medoxomil, Chlorthalidone and Cilnidipine

2020 ◽  
pp. 1-10
Author(s):  
Pranavkumar Shah ◽  
Bhavin Dhadhuk
Keyword(s):  
High Performance Liquid Chromatography ◽  
Liquid Chromatography ◽  
Mobile Phase ◽  
High Performance ◽  
Olmesartan Medoxomil ◽  
Drug Combinations ◽  
Column Temperature ◽  
Related Impurities ◽  
Limit Of Quantitation ◽  
Run Time

The liquid chromatography mass spectrometry (LC-MS) compatible, stability-indicating, specific, linear, accurate, sensitive with less run-time related impurities reversed phase high-performance liquid chromatography (RP-HPLC) related impurities method has been developed for olmesartan medoxomil (OLM), chlorthalidone (CHLR), and cilnidipine (CIL) drug combinations, and the method has been validated according to ICH and US-FDA guidelines. The chromatographic separation was performed by using Hypersil-BDS Thermo-Scientific, C18 (12.5 cm, 4.6 mm, 5 microns particle size) column. Mobile phase-A was prepared by mixing 3.85 gm ammonium acetate in HPLC water and adjust pH 5.0 by using diluted acetic acid. Acetonitrile was taken as mobile phase-B. Initial mobile phase ratio (55:45 v/v) was adjusted for mobile phase-A: mobile phase-B followed by gradient program. Other chromatographic conditions such as column temperature 25 degrees, flow rate 1.0 mL/minutes with the detection wavelength at 260 nm. The retention time for CHLR impurity A, olmesartan (OL), OLM impurity A, were found about 2.7, 3.3, and 7.2 minutes respectively, with a total run time of 18.0 minutes. The linearity calibration plot was performed and found linear relationship over the concentration range of 1.25 limit of quantitation (LoQ)–18.75 μg/mL, 3.6 LoQ–60.0 μg/mL, 3.6 LoQ–60.0 μg/mL respectively for CHLR impurity A, OL and OLM impurity A respectively. The limit of detection (LoD) and LoQ were found 0.4 ppm (μg/mL) and 1.2 ppm (μg/mL), 1.2 ppm (μg/mL) and 3.5 ppm (μg/mL), 1.1 ppm (μg/mL) and 3.3 ppm (μg/mL) for CHLR impurity A, OL and OLM impurity A respectively. The accuracy was determined by recovery studies and was found between 90.0–110.0%. The developed analytical method has been validated for LoD-LoQ, specificity, linearity, accuracy, precision, robustness, and ruggedness, which were well within the acceptance limit as per ICH guidelines. All the degradation products generated by stress conditions were found to be well separated from one another (all drug components and impurities). The developed method with shorter runtime was successfully implemented for routine quality control and stability analysis to check the quality of OLM, CHLR, and CIL drug combinations.

scholarly journals Analisis Beberapa Asam Organik dengan Metode High Performance Liquid Chromatography (HPLC) Grace Smart Rp 18 5µ

Jurnal MIPA ◽  
2015 ◽  
Vol 4 (2) ◽  
pp. 148
Author(s):  
Lungguk Sitorus ◽  
Julius Pontoh ◽  
Vanda Kamu
Keyword(s):  
Ascorbic Acid ◽  
High Performance Liquid Chromatography ◽  
Acetic Acid ◽  
Mobile Phase ◽  
High Performance ◽  
Potassium Dihydrogen Phosphate ◽  
Hplc Method ◽  
Dihydrogen Phosphate ◽  
Column Temperature ◽  
Potassium Dihydrogen

Metode HPLC fase terbalik dengan kolom Grace Smart RP 18 5µ dapat digunakan untuk memisahkan dan menentukan konsentrasi asam-asam organik. Metode ini diaplikasikan suhu kolom 40 oC dan dideteksi pada panjang gelombang 210 nm dengan kalium dihidrogenfosfat (pH 2,8) sebagai fase gerak. Metode ini telah digunakan untuk menentukan asam-asam organik seperti asam malat, asam askorbat, asam laktat, asam asetat, asam sitrat, asam piroglutamat, dan asam fumarat.Reverse phase HPLC method using Grace smart RP 18 5µ can used to separating and calculating concentration of organic acid. This method did on 40 0C column temperature and detected on wavelength 210 nm with potassium dihydrogen phosphate (pH 2.8) as mobile phase. Determining of organic acids such as malic acid, ascorbic acid, lactic acid, acetic acid, citric acid, pyroglutamic acid and fumaric acid.

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