Isoquinoline alkaloids and keto-fatty acids of Argemone ochroleuca and A. mexicana (mexican poppy) seed. I. An assay method and factors affecting their concentration

1993 ◽  
Vol 44 (2) ◽  
pp. 265 ◽  
Author(s):  
MT Fletcher ◽  
G Takken ◽  
BJ Blaney ◽  
V Alberts
Keyword(s):  
High Performance ◽  
Seed Oil ◽  
Assay Method ◽  
Crystalline Solid ◽  
Lauryl Sulfate ◽  
Isoquinoline Alkaloids ◽  
Poppy Seed ◽  
Factors Affecting ◽  
Place Of Origin ◽  
Total Alkaloid Content

An assay for the isoquinoline alkaloids of Argemone ochroleuca and A. mexicana seeds is described. The method consists of extraction into weakly acidified methanol and ion-pair high performance liquid chromatography with sodium lauryl sulfate and tartaric acid in acetonitri1e:water as eluent. Analysis of A. ochroleuca seed showed it to contain dihydrosanguinarine and dihydrochelerythrine (c. 3 : 2) as major alkaloid components with minor amounts of protopine, sanguinarine, berberine and chelerythrine. A single sample of authenticated A. mexicana seed contained dihydrosanguinarine as the major alkaloid with minor amounts of sanguinarine and berberine, in agreement with earlier studies. Dihydrosanguinarine and dihydrochelerythrine were measured as their oxidized products, sanguinarine and chelerythrine, after U.V. irradiation. A crystalline solid which separates from A. ochroleuca seed oil was shown to contain 11-oxo-octacosanoic acid and 11-oxo-triacontanoic acid, which are also the major components of a similar solid from A. mexicana seed oil. Mexican poppy seed (probably A. ochroleuca) collected from various regions of Queensland during 1987-89 showed that place of origin and length of storage of intact seed had little effect on alkaloid levels. Exposure of crushed seed to light, however, caused a rapid decrease in the concentration of dihydro-alkaloids. Total alkaloid content correlated with seed maturity, with immature seed containing much less than mature seed.

Development of Validated Stability Indicating HPTLC Method for Assay of Ozagrel and its Pharmaceutical Formulations

2018 ◽  
pp. 36-48 ◽  
Author(s):  
Vishal N Kushare ◽  
Sachin S Kushare
Keyword(s):  
High Performance ◽  
Linear Regression Analysis ◽  
Pharmaceutical Formulations ◽  
Base Hydrolysis ◽  
Assay Method ◽  
Related Substance ◽  
Stability Indicating ◽  
Regular Production ◽  
Hptlc Method

The present paper describes stability indicating high-performance thin-layer chromatography (HPTLC) assay method for Ozagrel in bulk drugs. The method employed TLC aluminium plates precoated with silica gel 60F-254 as the stationary phase. The solvent system consisted of toluene: methanol: triethylamine (6.5: 4.0: 0.1 v/v/v). The system was found to give compact spot for Ozagrel (Rf value of 0.40 ± 0.010). Densitometric analysis of Ozagrel was carried out in the absorbance mode at 280 nm. The linear regression analysis data for the calibration plots showed good linear relationship with r2 = 0.999 with respect to peak area in the concentration range 30 - 120 ng/spot. The developed HPTLC method was validated with respect to accuracy, precision, recovery and robustness. Also to determine related substance and assay determination of Ozagrel that can be used to evaluate the quality of regular production samples. The developed method can also be conveniently used for the assay determination of Ozagrel in pharmaceutical formulations. The limits of detection and quantitation were 4.069 and 12.332 ng/spot, respectively by height. Ozagrel was subjected to acid and alkali hydrolysis, oxidation, photochemical and thermal degradation. The drug undergoes degradation under acidic, basic, oxidation and heat conditions. This indicates that the drug is susceptible to acid, base hydrolysis, oxidation and heat. Statistical analysis proves that the method is repeatable, selective and accurate for the estimation of said drug. The proposed developed HPTLC method can be applied for identification and quantitative determination of Ozagrel in bulk drug and tablet formulation.

Reversed-Phase High Performance Liquid Chromatographic Analysis of Three First Line Anti-Tuberculosis Drugs

2019 ◽  
Vol 69 (12) ◽  
pp. 3590-3592
Author(s):  
Nela Bibire ◽  
Romeo Iulian Olariu ◽  
Luminita Agoroaei ◽  
Madalina Vieriu ◽  
Alina Diana Panainte ◽  
...  
Keyword(s):  
High Performance ◽  
Biological Fluids ◽  
Gradient Elution ◽  
High Performance Liquid Chromatographic ◽  
Reversed Phase ◽  
Assay Method ◽  
Active Pharmaceutical Ingredients ◽  
First Line ◽  
Pharmaceutical Ingredients ◽  
Liquid Chromatographic

Active pharmaceutical ingredients such as isoniazid, pyrazinamide and rifampicin are among the most important first-line anti-tuberculosis drugs. A simple, rapid and sensitive reversed phase-high performance liquid chromatographic assay method for the simultaneous determination of isoniazid, pyrazinamide and rifampicin has been developed. Separation of the interest compounds was achieved in a 10 min chromatographic run in gradient elution mode on a Zorbax SB-C18 stainless steel column (150 � 4 mm, 5 mm) using a guard column containing the same stationary phase. The gradient elution was carried out with a mobile phase of 10% CH3CN aqueous solution for channel A and 50% CH3CN in pH = 6.8 phosphate buffer (20 mM), to which 1.5 mL triethylamine were added for channel B. Quantification of the analyzed substances was carried out spectrophotometrically at 269 nm. Detection limits of 0.48 mg/L for isoniazid, 0.52 mg/L for pyrazinamide and 0.48 mg/L for rifampicin were established for the developed assay method. The present work showed that the proposed analysis method was advantageous for simple and rapid analysis of the active pharmaceutical ingredients in pharmaceuticals and biological fluids.

Bioanalytical method development and validation of simultaneous analysis of telmisartan and hydrochlorthiazide in human plasma using LC-MS/MS

2016 ◽  
Vol 5 (03) ◽  
pp. 4862 ◽  
Author(s):  
Mathew George* ◽  
Lincy Joseph ◽  
Arpit Kumar Jain ◽  
Anju V.
Keyword(s):  
Human Plasma ◽  
Retention Time ◽  
High Performance ◽  
Method Development ◽  
Matrix Effects ◽  
Solid Phase ◽  
Internal Standard ◽  
Assay Method ◽  
Buffer System ◽  
Internal Standards

A simple, sensitive, rapid and economic high performance thin layer chromatographic method and a mass spectroscopic assay method has been developed for the quantification of telmisartan and hydrochlorthiazide combination in human plasma. The internal standards and analytes were extracted from human plasma by solid-phase extraction with HLB Oasis1cc (30mg) catridges. The scanning and optimization for the samples are done using methanol: water (50:50). The samples were chromatographed using reverse phase chromatography with C-18 column of different manufacturers like Ascentis C18 (150×4. 6, 5µ) using the buffer system Acetonitrile: Buffer (80:20%v/v) which consist of 2±0. 1Mm ammonium format at a flow rate of 0. 7ml/min at a column oven temperature 35±10c. The internal standard used was hydrochlorthiazide13c1, d2 and telmisartand3. The extraction techniques include conditioning, loading, washing and elution, drying followed by reconstitution of the dried samples. The volume injected was 10µl with the retention time of 3-4 min for telmisartan, 1-2 min for hydrochlorthiazide and for the internal standards the retention time was 3-4 min for telmisartand3 and 1-2 min for hydrochlorthiazide c13d2. The rinsing solution was Acetonitrile: HPLC grade water in the ratio (50:50). The above developed method was validated using various parameters like selectivity and sensitivity, accuracy and precision, matrix effects, % recovery and various stability studies. The method was proved to be sensitive, accurate, precise and reproducible. The preparation showed high recovery for the quantitative determination of telmisartan and hydrochlorthiazide in human plasma.

scholarly journals Evaluation of the Bioactive Compounds Found in Tomato Seed Oil and Tomato Peels Influenced by Industrial Heat Treatments

Foods ◽  
2021 ◽  
Vol 10 (1) ◽  
pp. 110
Author(s):  
Katalin Szabo ◽  
Francisc Vasile Dulf ◽  
Bernadette-Emőke Teleky ◽  
Panagiota Eleni ◽  
Christos Boukouvalas ◽  
...  
Keyword(s):  
Fatty Acid ◽  
High Performance ◽  
Seed Oil ◽  
Edible Oils ◽  
Action Plan ◽  
Syringic Acid ◽  
Tomato Seed ◽  
Tomato Processing ◽  
Main Fatty Acid ◽  
Tomato Seed Oil

The circular economy action plan involves principles related to food waste reduction and integration of recovered nutrients to the market. In this context, the present study aims to highlight the valuable bioactive components found in tomato processing by-products (carotenoids, phenolic compounds and fatty acids) influenced by industrial pre-treatments, particularly cold break (CB) process at 65–75 °C and hot break (HB) process at 85–95 °C. The fatty acid profile of the tomato seed oil was examined by gas chromatography coupled to mass spectrometry (GC-MS), individual carotenoid and phenolic compositions were determined by high performance liquid chromatography (HPLC) and the viscoelastic properties were evaluated by rheological measurements. The physicochemical properties revealed appropriate characteristics of the tomato seed oil to fit the standards of generally accepted edible oils, for both CB and HB derived samples, however, significant qualitative and quantitative differences were detected in their phenolic composition and carotenoids content. Lycopene (37.43 ± 1.01 mg/100 mL) was a major carotenoid in the examined samples, linoleic acid was the main fatty acid (61.73%) detected in the tomato seed oil and syringic acid appeared to be one of two major phenolic acids detected in the samples of CB process. Our findings extend the boundaries of tomato processing industry by validating that tomato seed oil is a bioactive rich edible oil with additional health benefits, which can be integrated in functional food products.

scholarly journals Investigation of the oil and Meal of Japanese Quince (Chaenomeles Japonica) Seeds

2013 ◽  
Vol 67 (4-5) ◽  
pp. 405-410 ◽  
Author(s):  
Inese Mierina ◽  
Rasma Seržaneļ ◽  
Maija Strele ◽  
Jūlija Moskaļuka ◽  
Elga Ivdre ◽  
...  
Keyword(s):  
High Performance ◽  
Seed Oil ◽  
Water Extract ◽  
Syringic Acid ◽  
Barley Grain ◽  
Butylated Hydroxytoluene ◽  
Synthetic Antioxidant ◽  
Japanese Quince ◽  
Comparable Activity ◽  
First Time

Abstract Various extracts of Japanese quince (Chaenomeles japonica) seeds obtained using organic solvents were studied for their polyphenol content and antiradical activity. It was established that petroleum ether, hexane, ethyl acetate, acetone, as well as toluene and chloroform extracts, in comparison to synthetic antioxidant butylated hydroxytoluene (BHT), demonstrate better (or comparable) activity against 2,2-diphenyl-1-picrylhydrazyl (DPPH). Methods for detoxification of seeds, meals and press-cakes are proposed. Phenolic composition of different extracts (80% ethanol, 70% acetone), both acid and alkali hydrolysates of seeds, as well as seed oil methanol/water extract were analysed by means of high performance liquid chromatography (HPLC): chlorogenic acid was found for the first time in seed extract; protocatechuic acid predominated in all extracts. The content of other major phenolic acids was detected; it was found that seed oil contains syringic acid. It was determined that Japanese quince seeds contain almost ten times more α -tocopherol than barley grain. Due to the presence of α -tocopherol and phenolic compounds, seed oil and lipophilic extracts of seeds could serve as antioxidants.

Novel Determination of Anti-Hypertensive Combination; Benidipine Hydrochloride and Nebivolol Hydrochloride by High Performance Chromatographic Method

2021 ◽  
pp. 5433-5438
Author(s):  
V.L.N. Balaji Gupta Tiruveedhi ◽  
Venkateswara Rao Battula ◽  
Kishore Babu Bonige ◽  
Tejeswarudu B.
Keyword(s):  
High Performance ◽  
Degradation Products ◽  
Research Work ◽  
Hplc Method ◽  
Assay Method ◽  
Injection Quantity ◽  
Relative Standard ◽  
Nebivolol Hydrochloride ◽  
Concentration Series

This research work was designed to establish and validate a novel stability indicating RP-HPLC method for the combined determination of Benidipine hydrochloride (BHE) and Nebivolol hydrochloride (NHE) in bulk and tablets, dependent on ICH guidelines.The assay method to analyse BHE and NHE was optimized with isocratic elution using acetonitrile: 0.1M acetate buffer (45:55, pH 5.1), Lichrospher ODS RP-18 column and flow pace of 1 ml/min. Total time for single run was 14 min. The injection quantity was 20μl, and was detected at 249nm. The method was verified on a concentration series of 1.25-10μg/ml (NHE) and 1.0-10μg/ml (BHE) for precision, accuracy and linearity. The LOD values were 0.059µg/ml and 0.028µg/ml for NHE and BHE, respectively. The LOQ values were 0.196µg/ml for NHE and 0.094µg/ml for BHE. The recovery percentages were 98.60-100.11% (BHE) and 98.94-101.50% (NHE) with relative standard deviation 0.250-0.694% (BHE) and 0.183-0.400% (NHE). The method was also observed to be efficient, and was sufficiently specific to measure BHE and NHE in the presence of stress-produced degradation products.

Factors Affecting Aflatoxin B1 Removal by Flavobacterium aurantiacum

1995 ◽  
Vol 58 (1) ◽  
pp. 91-94 ◽  
Author(s):  
J. E. LINE ◽  
R. E. BRACKETT
Keyword(s):  
High Performance Liquid Chromatography ◽  
Liquid Chromatography ◽  
Aflatoxin B1 ◽  
Spectrophotometric Method ◽  
Phosphate Buffer ◽  
High Performance ◽  
Hplc Method ◽  
Apparent Effect ◽  
Factors Affecting ◽  
Aflatoxin Concentration

This study was conducted to investigate several factors affecting the removal of aflatoxin B1 by Flavobacterium aurantiacum NRRL B-184. A simple spectrophotometric procedure was evaluated and compared to an established high-performance liquid chromatography (HPLC) method and found to be useful for determining aflatoxin concentration in test solutions of phosphate buffer. Using the spectrophotometric method, 72-h cultures of F. aurantiacum were observed to remove more toxin from solution than 24-h cultures. Likewise, populations of 1010cells removed aflatoxin at a faster rate than did 109 cells, although the total amount removed did not differ. Transferring F. aurantiacum cultures in tryptic soy broth every 3 days for over 3 days for over 8 months had no apparent effect on their ability to remove measurable amounts of aflatoxin B1 from solution. Populations of 1 × 109 CFU/ml or less heat-inactivated F. aurantiacum were unable to remove aflatoxin B1 from phosphate buffer.

scholarly journals METHYL 10-EPI-PHEOPHORBIDE A FROM MCF-7 CELLS ACTIVE LAYER OF THE INDONESIAN FICUS DELTOIDEA JACK LEAVES

2017 ◽  
Vol 9 (8) ◽  
pp. 183 ◽  
Author(s):  
Anggia Murni ◽  
Novriyandi Hanif ◽  
Masaki Kita ◽  
Latifah K. Darusman
Keyword(s):  
Active Layer ◽  
Column Chromatography ◽  
Breast Tumor ◽  
High Performance ◽  
Chemical Structure ◽  
High Resolution Mass Spectrometry ◽  
Assay Method ◽  
Pheophorbide A ◽  
Ficus Deltoidea ◽  
Mcf 7

Objective: To isolate and elucidate a cytotoxic principle against breast tumor MCF-7 cells of the Indonesian terrestrial plant Ficus deltoidea Jack leaves.Methods: F. deltoidea leaves collected at National Park of mount Gede-Pangrango, Indonesia have been subjected to chemical and biological work. F. deltoidea leaves were extracted with 96% aqueous ethanol (EtOH) and was then partitioned into three layers n-hexane, dichloromethane (CH2Cl2), and n-butanol (n-BuOH). All layers were checked for their activity against breast tumor MCF-7 cells using MTT assay method. A portion of the most active layer was purified using open column chromatography to give fraction that has toxicity against zebra fish embryos. Based on the assay-guided isolation, compound 1 was isolated. The chemical structure of 1 was elucidated using nuclear magnetic resonance (NMR) and high-resolution mass spectrometry (HRMS) data as well as comparing data with literature.Results: The CH2Cl2 layer of F. deltoidea leaves was found to inhibit breast tumor MCF-7 cells with IC50 10 µg/ml which was the most toxic among the layers. A portion of the most active layer was purified using open column chromatography to give 7 fractions. The fraction 5 showed toxicity against zebrafish embryos (LC50 35 µg/ml, 48 hpf). This fraction was purified using high performance liquid chromatography (HPLC) octadecylsilyl (ODS) column with gradient elution 70% aqueous acetonitrile (MeCN) to 100% MeCN (linear gradient) for 40 min with UV detection at 254 nm (tR = 30.99 min) to give compound 1. The chemical structure of 1 was revealed as a chlorin-type compound named methyl 10-epi-pheophorbide A.Conclusion: Methyl 10-epi-pheophorbide A was isolated for the first time from the active fraction of the Indonesian F. deltoidea leaves or tabat barito. The chemical structure including absolute stereo chemistry was elucidated using NMR and HRMS data as well as by comparison with the literature values. The 13C NMR data has been added to complete the previous report.

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