High-Performance Liquid Chromatography Quantitative Determination of Oxyresveratrol and Morin Contained in Maclura cochinchinensis Extract and Gel Formulation

2021 ◽  
Vol 901 ◽  
pp. 79-85
Author(s):  
Arpa Petchsomrit ◽  
Boonyadist Vongsak

Maclura cochinchinensis (Lour.) Corner., of the Moraceae family, is a medical shrub commonly found in Thailand, and for which a wide variety of pharmacological activities have been reported, including antiviral, anti-inflammatory, antioxidant, and anticancer activities. The main bioactive compounds, oxyresveratrol and morin, are known to be found in M. cochinchinensis heartwood. In this study, we quantitatively analyzed the levels of these two active substances in M. cochinchinensis extracted with various solvents, including in various cosmetic formulations and herbs sourced from various parts of Thailand. High-performance liquid chromatography (HPLC) was performed on a C18 column with an isocratic elution using 1.5% formic acid and acetonitrile at a flow rate of 1 ml/min, and detected at 352 nm. This method was validated for accuracy, precision, linearity, limits of detection, and quantification. The average percent recovery for oxyresveratrol and morin in the extracts was 100.01 ± 0.62% and 99.31 ± 2.56%, and in gel formulation was 99.65 ± 3.54% and 118.41 ± 4.70%, respectively. The relative standard deviation of intra- and inter-day precision was less than 2.0% and 2.8%, respectively. Limits of detection and quantification were 0.06 and 0.2 μg/ml, respectively. The amounts of oxyresveratrol and morin extracted from different solvents, such as acetone, 80% ethanol, 50% ethanol, methanol, and distilled water were in the range of 37.75–68.16 and 54.63–144.83 mg/g, respectively, while five samples of M. cochinchinensis heartwood collected from different regions of traditional drug stores contained in the range of 26.85–60.37 and 110.26–157.44 mg/g, respectively. Additionally, the percentage label amounts of oxyresveratrol and morin were analyzed in gel preparations, and found at 82.88% and 120.99%, respectively. This technique is convenient, simple, and reliable to effectively analyze the content of these active compounds in extracts and cosmetic products.

2015 ◽  
Vol 78 (6) ◽  
pp. 1226-1231 ◽  
Author(s):  
HYUN EE OK ◽  
SOO HYUN CHUNG ◽  
NARI LEE ◽  
HYANG SOOK CHUN

Aflatoxins B1, B2, G1, G2 (AFB1, AFB2, AFG1, AFG2), ochratoxin A (OTA), and zearalenone (ZEA) in dried and ground red pepper (Capsicum annuum) were simultaneously analyzed with high-performance liquid chromatography coupled to fluorescence detection after post–column derivatization. The analytical method was validated for specificity, selectivity, linearity, limits of detection and quantification, recovery, precision, and measurement of uncertainty. The limits of detection and quantification were 0.10 and 0.25 μg/kg for AFB1, 0.04 and 0.06 μg/kg for AFB2, 0.14 and 0.50 μg/kg for AFG1, 0.05 and 0.10 μg/kg for AFG2, 0.12 and 0.45 μg/kg for OTA, and 4.00 and 13.25 μg/kg for ZEA, respectively. The average recoveries ranged from 80.4 to 98.5% for different concentrations of AFB1, AFB2, AFG1, AFG2, OTA, and ZEA in spiked samples. The measurement uncertainties were 0.64 to 1.62 μg/kg for AFB1, 0.24 to 0.45 μg/kg for AFB2, 0.79 to 2.19 μg/kg for AFG1, 0.32 to 0.61 μg/kg for AFG2, 0.81 to 2.31 μg/kg for OTA, and 8.48 to 26.25 μg/kg for ZEA. This method was successfully applied for the simultaneous determination of mycotoxins for 78 red peppers collected from Korean and Indian markets. Aflatoxins (sum of AFB1, AFB2, AFG1, and AFG2) were detected in 2% of nonpacked samples (n = 23) and 43% of packed samples (n = 55), at levels of 0.04 to 38.03 μg/kg. OTA was detected in 4% of nonpacked samples and 48% of packed samples, at levels of 0.15 to 56.30 μg/kg. ZEA was not detected in any samples. These findings indicate that the analytical method described here is suitable for the routine determination of the amounts of AFs, OTA, and ZEA in dried and ground red pepper.


2006 ◽  
Vol 89 (6) ◽  
pp. 1552-1556
Author(s):  
ArmaĞan Önal ◽  
Olcay SaĞiri ◽  
S Müge Çetin ◽  
Sidika Toker

Abstract Reboxetine is used as a selective noradrenaline reuptake inhibitor for the treatment of major depressive disorders. It is effective in the treatment of severe depression and safer to use than traditional tricyclic antidepressants. In this study, a novel, simple, and rapid stability-indicating high-performance liquid chromatography (HPLC) method for reboxetine methansulfonate was successfully developed and validated for the assay of tablets. The method was used to quantify reboxetine in tablets; it employed a C18 column (150 4.6 mm id) with an isocratic mobile phase consisting of methanolphosphate buffer (pH 7, 0.02 M; 55 + 45, v/v) at a flow rate of 1.0 μmL/min. Reboxetine was detected by an ultraviolet detector at 277 nm. The retention time of reboxetine was about 4.5 min. The developed HPLC method was validated with respect to linearity, precision, sensitivity, accuracy, and selectivity. The method was linear over the concentration range 150 g/mL (r 0.9999). The limits of detection and the quantitation of reboxetine were 0.1 and 0.3 μg/mL, respectively. The relative standard deviation values for intraday and interday precision were 0.781.01 and 1.081.37%, respectively. Selectivity was validated by subjecting a stock solution of reboxetine to neutral, acid, and alkali hydrolysis, as well as oxidation, dry heat treatment, and photodegradation. The peaks of the degradation products did not interfere with the peak of reboxetine. The results indicated that the proposed method could be used in a stability assay. The proposed method was successfully applied to the determination of reboxetine in tablets. Excipients present in the tablets did not interfere with the analysis.


2012 ◽  
Vol 550-553 ◽  
pp. 1173-1176
Author(s):  
Hui Qing Sun ◽  
Yi Qiang Li ◽  
Guang Jun Xu ◽  
Xiao Zhen ◽  
Jin Li Xu ◽  
...  

Abstract. [Aims] A high performance liquid chromatography (HPLC) was presented for determination of fentin acetate residue in beet and soils. [Methods] Fentin acetate was extracted from beet plants and soils with hydrochloric acid and acetonitrile, followed by a second extraction in dichloromethane, purified by acid aluminium oxide with methanol eluting, then dissolved by concentration and dilution with acetoneitrile. A HPLC with UV detection at 220 nm and a Waters Sun FireTM-C18 column, which was eluted with methanol and 0.5% phosphoric acid aqueous solution and was used based on an external standard calibration curve. [Results] The results showed that the average recoveries were 88.4-95.6% for beet plants and 91.2-91.8% for soils. The relative standard deviations were 2.0-4.5% and 4.3-5.3% respectively. The minimum detectable level was 1.6×10-10g, the lowest detectable concentration was 0.02mg/kg. [Conclusions] The method is convenient and can meet the requirement of residual analysis and also provide reference for other crops.


2013 ◽  
Vol 448-453 ◽  
pp. 406-408
Author(s):  
Jing Liu ◽  
Xiao Na Ji ◽  
Qing Kai Ren ◽  
Sheng Shu Ai ◽  
Li Jun Wan ◽  
...  

We established a method fordetermination of nitrate in water by High Performance Liquid Chromatography(HPLC). The sample was analysed by HPLC-ADA and was quantitated by externalstandard method after being simply processed. This methd has the advantages ofhigh separation efficiency and fast analysis. The experiment result showed thatthe linearly dependent coefficient was0.994, the recovery rate was between 98.7%~105.7%,the relative standard deviation(RSD)wasless than 2.1 %, and the lowest detectable limit is 0.01ng (S/N=1.6).


Author(s):  
Muhammad Fawad Rasool ◽  
Umbreen Fatima Qureshi ◽  
Nazar Muhammad Ranjha ◽  
Imran Imran ◽  
Mouqadus Un Nisa ◽  
...  

AbstractTh accurate rapid, simple and selective reversed phase high performance liquid chromatography (RP-HPLC) has been established and validated for the determination of captopril (CAP). Chromatographic separation was accomplished using prepacked ODSI C18 column (250 mm × 4.6 mm with 5 μm particle size) in isocratic mode, with mobile phase consisting of water: acetonitrile (60:40 v/v), pH adjusted to 2.5 by using 85% orthophosphoric acid at a flow rate of 1 mL/min and UV detection was performed at 203 nm. RP-HPLC method used for the analysis of CAP in mobile phase and rabbit plasma was established and validated as per ICH-guidelines. It was carried out on a well-defined chromatographic peak of CAP was established with a retention time of 4.9 min and tailing factor of 1.871. The liquid–liquid extraction method was used for extraction of CAP from the plasma. Excellent linearity (R2 = 0.999) was shown over range 3.125–100 µg/mL with mean percentage recoveries ranges from 97 to 100.6%. Parameters of precision and accuracy of the developed method meet the established criteria. Intra and inter-day precision (% relative standard deviation) study was also performed which was less than 2% which indicate good reproducibility of the method. The limit of detection (LOD) and quantification for the CAP in plasma were 3.10 and 9.13 ng/mL respectively. The method was suitably validated and successfully applied to the determination of CAP in rabbit plasma samples.


1982 ◽  
Vol 65 (6) ◽  
pp. 1395-1402
Author(s):  
Frank L Joe ◽  
Jean Salemme ◽  
Thomas Fazio

Abstract A simple, rapid method has been developed for the separation and determination of polynuclear aromatic hydrocarbons (PAHs) in barley malt. An ultrasonic- cyclohexane extraction method was used to separate the PAHs from ground barley malt. The cyclohexane extracts were purified by chromatography through a water-deactivated silica gel-alumina column. The eluate from the column was concentrated and purified further by partitioning between dimethyl sulfoxide (DMSO) and cyclohexane. The DMSO extract was diluted with water and the PAHs were extracted back into cyclohexane. The cyclohexane extract was washed with water, dried through sodium sulfate, and evaporated, and the resulting residue was dissolved in 80% aqueous acetonitrile-methanol (1 + 1) and subjected to reverse phase high performance liquid chromatography. Thirty barley malt samples were analyzed using this procedure. Peaks having the same retention time as the carcinogen benzo(a)pyrene were isolated from 18 of the samples, and were equivalent to trace levels ranging from <0.1 to 0.2 ppb. Average recoveries of 11 PAHs, including benzo(a)pyrene, benzo(b)fluoranthene, indeno(l,2,3-cd)pyrene, and benz(a)anthracene, added to 25 g samples at 2.5 and 5 ppb, ranged from 78 to 97%, with a mean relative standard deviation of 6.6%.


2020 ◽  
Vol 103 (5) ◽  
pp. 1223-1229
Author(s):  
Michikazu Tanio ◽  
Toru Nakamura ◽  
Hideki Kusunoki ◽  
Kyohei Ideguchi ◽  
Kazuyuki Nakashima ◽  
...  

Abstract Background Histamine fixed-immunoglobulin formulations, which consisted of 0.15 µg of histamine dihydrochloride and 12 mg of human immunoglobulin in a vial, are used for anti-allergic treatments, and controlling the amounts of histamine in the formulations is essential to avoid histamine intoxication. Objective A high-performance liquid chromatography (HPLC) method for determination of histamine contents of the formulations was established and validated. Methods Histamine extracted from the formulation was labeled with 6-aminoquinolyl-N-hydroxysuccinimidyl carbamate and was analyzed by gradient elution HPLC with UV detection at 260 nm. Results The method showed linearity in the range 0.8–2.4 µM (R > 0.999), accuracy (100.1–105.8% recovery), and precision (relative standard deviation ≤ 1.93%). The validated method was applied for five lots of the pharmaceutical, and their histamine contents were determined to be 0.149–0.155 µg/vial. Conclusions These results indicated that the validated method is useful to control amounts of histamine in biopharmaceutical products. Highlights The HPLC method was developed for quantitative determination of histamine content of the histamine fixed-immunoglobulin formulations.


2011 ◽  
Vol 47 (2) ◽  
pp. 363-371 ◽  
Author(s):  
Ananda Lima Sanson ◽  
Suéllen Cristina Rennó Silva ◽  
Matheus Coutinho Gonçalves Martins ◽  
Alexandre Giusti-Paiva ◽  
Patrícia Penido Maia ◽  
...  

A liquid-liquid extraction (LLE) combined with high-performance liquid chromatography-diode array detection method for simultaneous analysis of four chemically and structurally different antineoplastic drugs (cyclophosphamide, doxorubicin, 5-fluorouracil and ifosfamide) was developed. The assay was performed by isocratic elution, with a C18 column (5 µm, 250 x 4.6 mm) and mobile phase constituted by water pH 4.0- acetonitrile-methanol (68:19:13, v/v/v), which allowed satisfactory separation of the compounds of interest. LLE, with ethyl acetate, was used for sample clean-up with recoveries ranging from 60 to 98%. The linear ranges were from 0.5 to 100 µg mL-1, for doxorubicin and 1 to 100 µg mL-1, for the other compounds. The relative standard deviations ranged from 5.5 to 17.7%. This method is a fast and simple alternative that can be used, simultaneously, for the determination of the four drugs in plasma, with a range enabling quantification of the drugs in pharmacokinetics, bioequivalence and therapeutic drug-monitoring studies.


2011 ◽  
Vol 17 (1) ◽  
pp. 25-31 ◽  
Author(s):  
Bilal Yilmaz ◽  
Kadem Meral ◽  
Ali Asci ◽  
Yavuz Organer

In this study, a new and rapid spectrofluorometry and high performance liquid chromatography (HPLC) methods were developed for determination of metoprolol in pure and pharmaceutical dosage forms. The solvent system, wavelength of detection and chromatographic conditions were optimized in order to maximize the sensitivity of both the proposed methods. The linearity was established over the concentration range of 50-4000 ng ml-1 for spectrofluorometry and 5.0-300 ng ml-1 for HPLC methods. The intra- and inter-day relative standard deviation (RSD) was less than 4.14 and 3.86% for spectrofluorometry and HPLC, respectively. Limit of quantitation was determined as 30 and 5.0 ng ml-1 for spectrofluorometry and HPLC, respectively. No interference was found from tablet excipients at the selected assay conditions. The methods were applied for the quality control of commercial metoprolol dosage forms to quantify the drug and to check the formulation content uniformity.


2012 ◽  
Vol 577 ◽  
pp. 69-72 ◽  
Author(s):  
Shu Yu Liu ◽  
Anaerguli Maihemuti

A simple and rapid high performance liquid chromatography (HPLC) assay was developed to identify and measure theβ-sitosterol with chemical course and material applications in jatropha seed oil. The stigmasterol was isolated with a good selectivity by HPLC employing reversed phase C18 columns. The components were separated by mobile phase of methanol-water (99/1, v/v) and detected at 205nm. The quantitation of the stigmasterol was reproducible and the method relative standard deviation is 1.1%. The mean analytical recovery was 96.2%.


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