Development of a Sensitive High-Performance Liquid Chromatographic Method with Simple Extraction for Simultaneous Determination of Huperzine A and Huperzine B in the Species Containing Lycopodium Alkaloids

2009 ◽  
Vol 92 (4) ◽  
pp. 1060-1063 ◽  
Author(s):  
Yanqing Zhang ◽  
Junbo Xie ◽  
Wen-Qian Chen ◽  
Tian-Yan Zhou ◽  
Wei Lu
Keyword(s):  
Simultaneous Determination ◽  
High Performance ◽  
High Performance Liquid Chromatographic ◽  
Reversed Phase ◽  
Hplc Method ◽  
Huperzine A ◽  
Array Detector ◽  
Aqueous Acetic Acid ◽  
Simple Extraction

Abstract A sensitive HPLC method with simple extraction was developed for simultaneous determination of huperzine A (HupA) and huperzine B (HupB) in Huperzia serrata, H. crispata, H. miyoshiana, and Lycopodiastrum casuarinoides. In order to avoid conventional multiple-step and time-consuming sample preparation methods, direct reflux extraction with alkaline chloroform was adopted. The quantitative determination was conducted by reversed-phase HPLC with a photodiode array detector set at 308 nm. Separation was performed on a Luna C18 column (250 4.6 mm id, 5 m) with methanol0.2 aqueous acetic acid (18 + 82, v/v) mobile phase. The method was validated for accuracy, reproducibility, precision, and limits of detection and quantification. Quantification of the two active compounds in the samples was performed by this newly developed method, and the content of HupA and HupB varied substantially among four different species. The satisfactory results indicated that the developed method can readily be utilized for quality control of the species of Huperziaceae and Lycopodiaceae containing the two compounds.

Development and Validation of a High Performance Liquid Chromatographic Method for Simultaneous Determination of Vitamins A and D3 in Fluid Milk Products

2015 ◽  
Vol 98 (2) ◽  
pp. 390-396 ◽  
Author(s):  
Yang Chen ◽  
Ravinder M Reddy ◽  
Wenjing Li ◽  
Ramesh R Yettlla ◽  
Salvador Lopez ◽  
...  
Keyword(s):  
Simultaneous Determination ◽  
High Performance ◽  
High Performance Liquid Chromatographic ◽  
Hplc Method ◽  
Array Detector ◽  
Technology Standard ◽  
Development And Validation ◽  
Liquid Chromatographic ◽  
Fluid Milk

Abstract An HPLC method for simultaneous determination of vitamins A and D3 in fluid milk was developed and validated. Saponification and extraction conditions were studied for optimum recovery and simplicity. An RP HPLC system equipped with a C18 column and diode array detector was used for quantitation. The method was subjected to a single-laboratory validation using skim, 2% fat, and whole milksamples at concentrations of 50, 100, and 200% of the recommended fortification levels for vitamins A and D3 for Grade “A” fluid milk. The method quantitation limits for vitamins A and D3 were 0.0072 and 0.0026 μg/mL,respectively. Average recoveries between 94 and 110%and SD values ranging from 2.7 to 6.9% were obtainedfor both vitamins A and D3. The accuracy of the method was evaluated using a National Institute of Standards and Technology standard reference material (1849a) and proficiency test samples.

scholarly journals Development and Validation of HPLC Method for Simultaneous Determination of Ceftriaxone and Cefaclor in Commercial Formulations and Biological Samples

2017 ◽  
Vol 57 (4) ◽  
Author(s):  
Jasmin Shah ◽  
M. Rasul Jan ◽  
Sultan Shah ◽  
M. Naeem Khan
Keyword(s):  
Simultaneous Determination ◽  
Human Plasma ◽  
High Performance ◽  
Limit Of Detection ◽  
High Performance Liquid Chromatographic ◽  
Reversed Phase ◽  
Hplc Method ◽  
Limit Of Quantification ◽  
Spiked Human Plasma

A reversed phase high performance liquid chromatographic method has been developed for the simultaneous determination of cefaclor and ceftriaxone cephalosporin antibiotic. The developed method has been validated and applied to mixtures of the commercial formulation and spiked human plasma. A mediterranea C<sub>18</sub> column (4.6 × 250 mm) was used with isocratic solvent delivery system and UV-visible detector. Different experimental parameters like solvent composition (acetonitrile: methanol: triethyl amine buffer 1:1:2 (v/v), flow rate of mobile phase (0.6 mLmin<sup>-1</sup>), pH of the buffer (7), and wavelength (260 nm) were optimized for effective separation and esolution of the analyte peaks. The separation was achieved in 6 min with retention times of 4.94 ± 0.056 min and 3.39 ± 0.022 min for cefaclor and ceftriaxone respectively. The linear range for both the studied drugs was found to be 0.5-250 μgmL<sup>-1</sup> with r<sup>2</sup> of 0.9987 (cefaclor) and 0.9997 (ceftriaxone). The limit of detection (3.3 σ/S) was found to be 2.34 × 10<sup>-2</sup> μgmL−1 and 1.70 × 10−2 μgmL<sup>-1</sup>, respectively, for cefaclor and ceftriaxone. Similarly limit of quantification (10σ/S) was 7.10 × 10−2 μgmL<sup>-1</sup> for cefaclor and 5.15 × 10−2 μgmL<sup>-1</sup> for ceftriaxone. The chromatographic procedure was applied to commercial formulations and spiked human plasma and the results were compared with literature HPLC method.

scholarly journals Simultaneous Determination of Preservatives (Methyl Paraben and Propyl Paraben) in Sucralfate Suspension Using High Performance Liquid Chromatography

2011 ◽  
Vol 8 (1) ◽  
pp. 340-346 ◽  
Author(s):  
Rajesh M. Kashid ◽  
Santosh G. Singh ◽  
Shrawan Singh
Keyword(s):  
High Performance Liquid Chromatography ◽  
Simultaneous Determination ◽  
Mobile Phase ◽  
High Performance ◽  
Reversed Phase ◽  
Hplc Method ◽  
Reversed Phase Hplc ◽  
Methyl Paraben ◽  
Propyl Paraben

A reversed phase HPLC method that allows the separation and simultaneous determination of the preservatives methyl paraben (M.P.) and propyl paraben (P.P.) is described. The separations were effected by using an initial mobile phase of water: acetonitrile (50:50) on Inertsil C18 to elute P.P. and M.P. The detector wavelength was set at 205 nm. Under these conditions, separation of the two components was achieved in less than 10 min. Analytical characteristics of the separation such as precision, specificity, linear range and reproducibility were evaluated. The developed method was applied for the determination of preservative M.P. and P.P. at concentration of 0.01 mg/mL and 0.1 mg/mL respectively. The method was successfully used for determining both compounds in sucralfate suspension.

Development and validation of a fast and simple HPLC method for the simultaneous determination of aniline and its degradation products in wastewater

2016 ◽  
Vol 8 (30) ◽  
pp. 5949-5956 ◽  
Author(s):  
Soumia Boulahlib ◽  
Ali Boudina ◽  
Kahina Si-Ahmed ◽  
Yassine Bessekhouad ◽  
Mohamed Trari
Keyword(s):  
High Performance ◽  
Degradation Products ◽  
Reversed Phase ◽  
Hplc Method ◽  
Array Detector ◽  
Simple Method ◽  
Photodiode Array Detector ◽  
Photodiode Array ◽  
Development And Validation

In this study, a rapid and simple method based on reversed-phase high performance liquid chromatography (RP-HPLC) using a photodiode array detector (PDA) for the simultaneous analysis of five pollutants including aniline and its degradation products, para-aminophenol, meta-aminophenol, ortho-aminophenol and phenol, was developed.

scholarly journals Simultaneous determination of clobutinol hydrochloride and doxylamine succinate from syrups by RP HPLC using a new stationary phase containing embedded urea polar groups

2012 ◽  
Vol 48 (2) ◽  
pp. 315-323 ◽  
Author(s):  
Paulo Cesar Pires Rosa ◽  
Isabel Cristina Sales Fontes Jardim
Keyword(s):  
Stationary Phase ◽  
Simultaneous Determination ◽  
Reversed Phase ◽  
Hplc Method ◽  
Array Detector ◽  
Polar Groups ◽  
Ich Guidelines ◽  
Relative Standard ◽  
New Stationary Phase

A new, simple, fast, reproducible and sensitive reversed phase HPLC method, using a new stationary phase containing embedded urea polar groups, has been developed and validated for the simultaneous determination of clobutinol hydrochloride (CLO) and doxylamine succinate (DOX) in syrups. The determination was carried out on a C8 urea column (125 mm x 3.9 mm i.d., 5 µm particle size) synthetized at the Liquid Chomatography Laboratory (LabCrom) of the Chemistry Institute of Unicamp. The mobile phase consisted of a mixture of acetonitrile:methanol:phosphate buffer (pH 2.5) in the gradient mode. The diode array detector (DAD) was operated at 230 nm for CLO and 262 nm for DOX. The method showed adequate precision, with relative standard deviations (RSD) less than 1%. The presence of the excipients did not interfere in the results of the analysis. Accuracy was determined by adding standards of the drugs to a placebo and good recovery values were obtained. The analytical curves were linear (r² 0.9999 for CLO and 0.9998 for DOX) over a wide concentration range (2.4-336 µg mL-1 for CLO and 2.3-63 µg mL-1 for DOX). The solutions were stable for at least 72 hours at room temperature. The criteria for validation using the ICH guidelines were fulfilled.

scholarly journals Determination of Dyclonine Hydrochloride by a HPLC Method and Camphor and Menthol by a GC Method in Compound Lotion

2013 ◽  
Vol 2013 ◽  
pp. 1-4
Author(s):  
Suying Ma ◽  
Haixia Lv ◽  
Xiaojun Shang
Keyword(s):  
Retention Time ◽  
High Performance ◽  
High Performance Liquid Chromatographic ◽  
Reversed Phase ◽  
Hplc Method ◽  
Ionization Detector ◽  
Uv Detector ◽  
Flame Ionization ◽  
Liquid Chromatographic

A high performance liquid chromatographic (HPLC) method with UV detector for the determination of dyclonine hydrochloride and a gas chromatography (GC) method with flame ionization detector (FID) for the determination of camphor and menthol in lotion were developed. The developed HPLC method involved using a SinoChoom ODS-BP C18reversed-phase column (5 μm, 4.6 mm × 200 mm) and mobile phase consisting of acetonitrile : water : triethylamine in a ratio of 45 : 55 : 1.0; pH was adjusted to 3.5 with glacial acetic acid. The developed GC method for determination of camphor and menthol involved using an Agilent 19091J-413 capillary chromatographic column (30 m × 320 μm × 0.25 μm). The two methods were validated according to official compendia guidelines. The calibration of dyclonine hydrochloride for HPLC method was linear over the range of 20–200 μg/mL. The retention time was found at 6.0 min for dyclonine hydrochloride. The calibration of camphor and menthol of GC method was linear over the range of 10–2000 μg/mL. The retention time was found at 2.9 min for camphor and 3.05 min for menthol. The proposed HPLC and GC methods were proved to be suitable for the determination of dyclonine hydrochloride, camphor, and menthol in lotion.

DEVELOPMENT AND VALIDATION OF A NEW RP HPLC METHOD FOR ROUTINE DETERMINATION OF TEA TREE OIL IN BULK AND COSMECEUTICAL FORMULATIONS

INDIAN DRUGS ◽  
2019 ◽  
Vol 56 (07) ◽  
pp. 43-49
Author(s):  
B.P. Manjula ◽  
V. G Joshi ◽  
Siddamsetty Ramachandra Setty ◽  
M Geetha ◽  
Keyword(s):  
High Performance ◽  
High Performance Liquid Chromatographic ◽  
Reversed Phase ◽  
Hplc Method ◽  
Tea Tree Oil ◽  
Tea Tree ◽  
Liquid Chromatographic Method ◽  
Development And Validation ◽  
Liquid Chromatographic

Tea tree oil, an active ingredient of skin, hair and nail care cosmeceuticals, has claims for topical antimicrobial, analgesic and anti-inflammatory activity. Its complex composition is governed by ISO 4730:2017. Terpinene-4-ol is the principal constituent of the oil (35% - 48%) followed by γ-terpinene (14% -28%), α-terpinene (6%-12%) and 1,8-cineole (≤15%). A reversed-phase, isocratic high performance liquid chromatographic method has been developed and validated for routine determination of tea tree oil based on1,8-cineole content in bulk and commercially available cosmeceuticals using C18 column, methanol-water (70:30 v/v) as mobile phase and flow rate of 1mL/min. UV detection was done at 200 nm. Linearity of the method was established for 20-100μL/mL (R2 = 0.9992) with LOD, LOQ values of 0.5594 μL/mL and 5.5941μL/mL respectively. The % RSD values for robustness and precision were <1% and recovery ranged between 99.09-102.96%. The method was successfully applied for determination of 1,8-cineole content in cosmeceuticals.

scholarly journals Development of a New High-Performance Liquid Chromatographic Method for the Determination of Ceftazidime

2008 ◽  
Vol 91 (4) ◽  
pp. 739-743 ◽  
Author(s):  
Andréia de Haro Moreno ◽  
Hérida Regina Nunes Salgado
Keyword(s):  
High Performance ◽  
High Performance Liquid Chromatographic ◽  
Reversed Phase ◽  
Hplc Method ◽  
Calibration Graph ◽  
Raw Material ◽  
Relative Standard ◽  
Validation Parameters ◽  
Liquid Chromatographic

Abstract A rapid, accurate, and sensitive high-performance liquid chromatographic (HPLC) method was developed and validated for the determination of ceftazidime in pharmaceuticals. The method validation parameters yielded good results and included range, linearity, precision, accuracy, specificity, and recovery. The excipients in the commercial powder for injection did not interfere with the assay. Reversed-phase chromatography was used for the HPLC separation on a Waters C18 (WAT 054275; Milford, MA) column with methanolwater (70 + 30, v/v) as the mobile phase pumped isocratically at a flow rate of 1.0 mL/min. The effluent was monitored at 245 nm. The calibration graph for ceftazidime was linear from 50.0 to 300.0 g/mL. The values for interday and intraday precision (relative standard deviation) were &lt;1. The results obtained by the HPLC method were calculated statistically by analysis of variance. We concluded that the HPLC method is satisfactory for the determination of ceftazidime in the raw material and pharmaceuticals.

Simultaneous determination of vitamins A and E and carotenoids in plasma by reversed-phase HPLC in elderly and younger subjects

1993 ◽  
Vol 39 (11) ◽  
pp. 2229-2234 ◽  
Author(s):  
Z Zaman ◽  
P Fielden ◽  
P G Frost
Keyword(s):  
Simultaneous Determination ◽  
High Performance ◽  
Ammonium Acetate ◽  
Beta Carotene ◽  
High Performance Liquid Chromatographic ◽  
Solvent Mixture ◽  
Reversed Phase ◽  
Alpha Tocopherol ◽  
Elderly Subjects

Abstract A reversed-phase high-performance liquid-chromatographic method for the simultaneous determination of retinol, alpha-tocopherol, alpha-carotene, beta-carotene, cryptoxanthin, lutein/zeaxanthin, and lycopene is described. This method was applied to plasma measurements in healthy young and elderly subjects. The plasma, deproteinized with ethanol, is extracted twice with n-hexane. After evaporation, the residue is dissolved in 50 microL of tetrahydrofuran and made up to 200 microL with ethanol. Samples (50 microL) are injected onto a 250 x 4.6 mm column of 5-microns-particle Spherisorb ODS1 (Phase Separations) that had been equilibrated with solvent mixture A:B (90:10 by vol) [A = 100 mmol/L ammonium acetate in methanol: acetonitrile (80:20 by vol) and B = 100 mmol/L ammonium acetate in water] at 2 mL/min. The analytes are eluted by running a 12-min linear gradient to 100% A; solvent A is then maintained for 10 min. Intrabatch CVs were 2.3%, 3.3%, 2.8%, 3.6%, 3.6%, and 3.0% for retinol, alpha-tocopherol, lutein/zeaxanthin, cryptoxanthin, lycopene, and beta-carotene, respectively. The corresponding interbatch CVs were 4.9%, 5.8%, 12.3%, 6.5%, 8.0%, and 3.4%.

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