Ephedrine Analysis in Real Urine Sample via Solvent Bar Microextraction Technique Coupled with HPLC-UV and Chemometrics

2018 ◽  
Vol 15 (1) ◽  
pp. 24-31 ◽  
Author(s):  
Persia Behbahani ◽  
Mahnaz Qomi ◽  
Nahid Ghasemi ◽  
Kambiz Tahvildari
Keyword(s):  
Urine Sample ◽  
High Performance ◽  
Limit Of Detection ◽  
Cost Effective ◽  
Cost Effective Method ◽  
Relative Standard ◽  
Designed Experiment ◽  
Preconcentration Factor ◽  
Beta Adrenergic Agonist ◽  
Solvent Bar Microextraction

Background: Ephedrine, an alpha/beta-adrenergic agonist, is one of the most common doping agents not only among athletes but also the ordinary people, therefore its detection at low trace levels with a sensitive and cost effective method has become a priority to investigate many analytical methods. Objective: In this work, solvent bar microextraction followed by high-performance liquid chromatography (HPLC-UV) was used for extraction and determination of ephedrine at low trace levels from urine samples at optimum condition. Methods: In this study, a designed experiment was carried out using solvent bar microextraction technique, which has been proved to be a green method. This method requires three phases consisting of a donor phase with an alkaline pH, an acceptor phase with an acidic pH, and organic solvent to impregnate the pores of the hollow fiber. The obtained results were used for estimating the optimum ranges for each parameter, analyzing the effect of different parameters, simultaneously. Results: Under optimized circumstances, the preconcentration factor was 129. The calibration curves represented good linearity for urine sample with coefficient estimations higher than 0.9991. The limit of detection and quantitation for ephedrine were 16.7 µg L-1 and 50 µg L-1, respectively. The relative standard deviations of analysis were 3.5% within a day (n=3) and 4.1% between days (n=9). Conclusion: According to the results and previous studies, it can be concluded that the preconcentration factor for ephedrine was the best result ever reported considering selectivity and cost-effectiveness.

Trace Determination of Tamoxifen using Optimized Solvent Bar Microextraction and HPLC-UV

2020 ◽  
Vol 16 (8) ◽  
pp. 1068-1073 ◽  
Author(s):  
Persia Behbahani ◽  
Nahid Ghasemi ◽  
Mahnaz Qomi ◽  
Kambiz Tahvildari
Keyword(s):  
High Performance ◽  
Limit Of Detection ◽  
Antineoplastic Agent ◽  
Hot Flashes ◽  
Limit Of Quantification ◽  
Dose Monitoring ◽  
Relative Standard ◽  
Preconcentration Factor ◽  
Set Up ◽  
Solvent Bar Microextraction

Background: Tamoxifen (Soltamox) is an antineoplastic agent and an estrogen receptor antagonist used to treat breast cancer, but have severe side effects such as hot flashes, vaginal discharge, etc. Dose monitoring is a necessity for optimum treatment, to prevent severe adverse effects. Methods: In this study, the solvent bar microextraction method (SBME) was used for preconcentration and microextraction coupled with High-performance liquid chromatography-ultraviolet (HPLC-UV) analysis of tamoxifen. Results: The limit of detection and limit of quantification were 13.3 and 40 μgL-1, respectively. The linear range was between 40 and 10000 μgL-1 with a correlation coefficient of 0.999. The enrichment factor was 169 and the relative standard deviation within-day and between-day were 3.6 and 4.0, respectively. Conclusion: The use of sensitive SBME method coupled with HPLC-UV analysis for detection of tamoxifen at trace level proved to be successful, offering a desirable preconcentration factor, and a costeffective and green set-up for determining its rate of elimination from cancer patients and wastewater.

Vortex-Assisted Dispersive Liquid–Liquid Microextraction Coupled with Deproteinization for Determination of Nateglinide in Human Plasma Using HPLC/UV

2020 ◽  
Author(s):  
Mohamed A Hammad ◽  
Amira H Kamal ◽  
Reham E Kannouma ◽  
Fotouh R Mansour
Keyword(s):  
Human Plasma ◽  
High Performance ◽  
Limit Of Detection ◽  
Signal To Noise Ratio ◽  
Cost Effective ◽  
Salt Addition ◽  
Relative Standard ◽  
Dispersive Liquid Liquid Microextraction ◽  
Liquid Microextraction

Abstract A validated method for preconcentration and determination of nateglinide in plasma was developed using vortex-assisted dispersive liquid–liquid microextraction. Different variables that affect extraction efficiency were studied and optimized, including type and volume of extractant, type and volume of disperser, pH of diluent, salt addition effect, centrifugation and vortex time. Nateglinide was extracted using 30 μL of 1-octanol as an extractant and 200 μL of methanol as a disperser. The enrichment factor reached 330 under the optimum conditions. High-performance liquid chromatography/ultraviolet was used for detection using phosphate buffer (pH 2.5, 10 mM): acetonitrile (45:55, v/v) as a mobile phase at a flow rate of 1 mL/min. The method was linear over the range of 50–20,000 ng/mL with a limit of detection of 15 ng/mL (signal-to-noise ratio = 3). Intra- and inter-day precision had %relative standard deviation <6% (n = 3) and the %recoveries were found to be between 102.5 and 105.9%. The proposed method is simple, sensitive, eco-friendly, cost-effective and powerful for microextraction of nateglinide from human plasma samples.

METHOD DEVELOPMENT AND VALIDATION OF OLANZAPINE IN PURE AND PHARMACEUTICAL DOSAGE FORM BY RP-HPLC METHOD

INDIAN DRUGS ◽  
2013 ◽  
Vol 50 (02) ◽  
pp. 20-26
Author(s):  
V.S Mastiholimath ◽  
◽  
P.M. Dandagi ◽  
A.P. Gadad ◽  
N.V Murali Krishna ◽  
...  
Keyword(s):  
High Performance ◽  
Dosage Form ◽  
Method Development ◽  
Limit Of Detection ◽  
Cost Effective ◽  
Hplc Method ◽  
Chromatography Method ◽  
Pharmaceutical Dosage Form ◽  
Relative Standard ◽  
Ammonium Hydrogen

A simple and reliable reverse phase high-performance liquid chromatography method was developed and validated for Olanzapine in pure and pharmaceutical dosage form. The method was developed on BDS Hypersil C18, (150 mm x 4.6 mm, 3μm) with a mobile phase of 0.01M tetra butyl ammonium hydrogen sulphate : methanol (80:20 v/v). The effluent was monitored by SPD-M20A, prominence UV-VIS detector at 234 nm. Calibration curve was linear over the concentration range of 10 –60μg/ml For interday and intraday precision % relative standard deviation values were found to be 0.18% and 0.24% respectively. Recovery of olanzapine was found to be in the range of 99.93 -100.00%. The limit of detection (LOD) and quantitation (LOQ) were 0.39275 and 1.1901μg/ml, respectively. The retention time and run time was very short; hence it is cost effective, making it more economical and rapid. Also this method can be used for the analysis of large number of samples.

scholarly journals Challenges of HPLC Method Development and Validation for the Assay of Bemotrizinol from Complex Matrix in Cosmeceutical Preparation

2020 ◽  
Vol 11 (03) ◽  
pp. 310-316
Author(s):  
Kallol S Jana ◽  
Beduin Mahanti
Keyword(s):  
Mobile Phase ◽  
High Performance ◽  
Method Development ◽  
Limit Of Detection ◽  
Linear Regression Analysis ◽  
Cost Effective ◽  
Analysis Data ◽  
Hplc Method ◽  
Limit Of Quantification ◽  
Relative Standard

A simple high performance liquid chromatography (HPLC) method was developed for the assay of bemotrizinol (Tinosorb-S) from the complex pharmaceutical cosmetics matrix. Unlike the existing methods, the proposed mobile phase used in this method is very simple and excluding buffer. The use of buffer reducing column longevity and also a time-consuming process which increases the cost of analysis. To overcome all the referred problems, the present article was developed and validated as per International Council for Harmonization (ICH) guidelines. The reverse-phase chromatography was performed on Shimadzu model no. SPD-M10A VP with LC solution software, μBondapack (3.9 × 300 mm, 10-micron particle size) column with methanol (100%) as mobile phase at a flow rate 2.5 mL per minutes and UV detection at 254 nm. The retention time of bemotrizinol was found in 17.599 minutes, and the linear regression analysis data for the calibration plots showed a good linear relationship in the concentration range 70 to 130 μg/mL. The value of the correlation coefficient, slope, and intercept were 0.996, 7,715, and 15,320, respectively. The limit of quantification (LoQ) and limit of detection (LoD) were found to be 1.32 and 0.44, respectively. The relative standard deviation (RSD) for intra-day sample A 1.0858, sample B 0.8859, and inter-day sample A 0.9921, sample B 0.967 which were found to be lesser than 2%. The developed method was validated with regard to linearity, accuracy, precision, selectivity, and robustness, and the method was found to be simple, cost-effective, precise, accurate, linear, and specific for the successful identification and determination of bemotrizinol in pharmaceutical cosmetic preparation.

Calcium/Copper alginate framework doped with CuO nano-particles as a novel adsorbent for micro-extraction of benzodiazepines from human serum

2020 ◽  
Vol 16 ◽  
Author(s):  
Nadereh Rahbar ◽  
Fatemeh Ahmadi ◽  
Zahra Ramezani ◽  
Masoumeh Nourani
Keyword(s):  
Human Serum ◽  
High Performance ◽  
Limit Of Detection ◽  
Solid Phase ◽  
Nano Particles ◽  
Limit Of Quantification ◽  
Analytical Methodology ◽  
Fiber Fabrication ◽  
Relative Standard ◽  
Green Procedure

Background: Sample preparation is one of the most challenging phases in pharmaceutical analysis, especially in biological matrices, affecting the whole analytical methodology. Objective: In this study, a new Ca(II)/Cu(II)/alginate/CuO nanoparticles hydrogel fiber (CCACHF) was synthesized through a simple, green procedure and applied for fiber micro solid phase extraction (FMSPE) of diazepam (DIZ) and oxazepam (OXZ) as model drugs prior to high-performance liquid chromatography-UV detection (HPLC-UV). Methods: Composition and morphology of the prepared fiber were characterized and the effect of main parameters on the fiber fabrication and extraction efficiency have been studied and optimized. Results: In optimal conditions, calibration curves were linear ranging between 0.1–500 µg L−1 with regression coefficients of 0.9938 and 0.9968. Limit of detection (LOD) (S/N=3) and limit of quantification (LOQ) (S/N=10) of the technique for DIZ and OXZ were 0.03 to 0.1 µg L−1. Within-day and between-day relative standard deviations (RSDs) for DIZ and OXZ were 6.0–12.5% and 3.3–9.4%, respectively. Conclusion: The fabricated adsorbent has been substantially employed to extraction of selected benzo-diazepines (BZDs) from human serum real specimens and the obtained recoveries were also satisfactory (82.1-109.7%).

scholarly journals Rapid Detection and Quantification of Patulin and Citrinin Contamination in Fruits

Molecules ◽  
2021 ◽  
Vol 26 (15) ◽  
pp. 4545
Author(s):  
Sudharsan Sadhasivam ◽  
Omer Barda ◽  
Varda Zakin ◽  
Ram Reifen ◽  
Edward Sionov
Keyword(s):  
High Performance ◽  
Cost Effective ◽  
Hplc Method ◽  
Pear Fruit ◽  
Cost Effective Method ◽  
Fruit Samples ◽  
Pome Fruits ◽  
Reliable Methods ◽  
By Products ◽  
Detection And Quantification

Patulin (PAT) and citrinin (CTN) are the most common mycotoxins produced by Penicillium and Aspergillus species and are often associated with fruits and fruit by-products. Hence, simple and reliable methods for monitoring these toxins in foodstuffs are required for regular quality assessment. In this study, we aimed to establish a cost-effective method for detection and quantification of PAT and CTN in pome fruits, such as apples and pears, using high-performance liquid chromatography (HPLC) coupled with spectroscopic detectors without the need for any clean-up steps. The method showed good performance in the analysis of these mycotoxins in apple and pear fruit samples with recovery ranges of 55–97% for PAT and 84–101% for CTN, respectively. The limits of detection (LOD) of PAT and CTN in fruits were 0.006 µg/g and 0.001 µg/g, while their limits of quantification (LOQ) were 0.018 µg/g and 0.003 µg/g, respectively. The present findings indicate that the newly developed HPLC method provides rapid and accurate detection of PAT and CTN in fruits.

Rapid and Sensitive Liquid Chromatographic Method for Determination of Anastrozole in Different Polymer–Lipid Hybrid Nanoparticles

2021 ◽  
pp. 247263032098230
Author(s):  
Dilshad Ahmad ◽  
Faisal A. Al Meshaiti ◽  
Yazeed K. Al Anazi ◽  
Osama Al Owassil ◽  
Alaa Eldeen B. Yassin
Keyword(s):  
High Performance ◽  
Limit Of Detection ◽  
Reversed Phase ◽  
Hplc Method ◽  
Hybrid Nanoparticles ◽  
Array Detector ◽  
Relative Standard ◽  
Validation Parameters ◽  
Limit Of Quantitation ◽  
Inhibitor Drug

Anastrozole, an aromatase inhibitor drug, is used for the treatment of breast cancer in pre- and postmenopausal women. Anastrozole’s incorporation into nanoparticulate carriers would enhance its therapeutic performance. To perceive the exact loaded amount of drug in nanocarriers, a valid analytical method is required. The reversed-phase high-performance liquid chromatography (RP-HPLC) method was developed and validated by using the C18 column, 150 × 4.6 mm, 5 µm particle size, in isocratic mobile phase composed of 50:50 V/V (volume/volume) acetonitrile–phosphate buffer (pH 3) flowing at a rate of 1.0 mL/min, and a diode array detector (DAD) set at λmax = 215 nm. The validation parameters such as linearity, accuracy, specificity, precision, and robustness have proven the accuracy of the method, with the relative standard deviation percentage (% RSD) values < 2. The limit of detection of the method was found equal to 0.0150 µg/mL, and the limit of quantitation was 0.0607 µg/mL. The percent recovery of sample was in the range of 98.04–99.25%. The method has the advantage of being rapid with a drug retention time of 2.767 min, specific in terms of resolution of peaks void of interference with any of the excipients, and high reproducibility. This makes it highly applicable for quality control purposes.

scholarly journals SENSITIVE DETERMINATION OF RELATED SUBSTANCES IN PIOGLITAZONE HYDROCHLORIDE BY HPLC

2017 ◽  
Vol 9 (2) ◽  
pp. 34
Author(s):  
N. Balaji ◽  
Sayeeda Sultana
Keyword(s):  
Mobile Phase ◽  
High Performance ◽  
Limit Of Detection ◽  
High Performance Liquid Chromatographic ◽  
Hplc Method ◽  
Internal Diameter ◽  
Related Substances ◽  
Relative Standard ◽  
Limit Of Quantitation

Objective: An efficient, high performance liquid chromatographic method has been developed and validated for the quantification of related substances in pioglitazone hydrochloride drug substance.Methods: This method includes the determination of three related substances in pioglitazone hydrochloride. The mobile phase A is 0.1% w/v triethylamine in water with pH 2.5 adjusted by dilute phosphoric acid. The mobile phase B is premixed and degassed mixtures of acetonitrile and methanol. The flow rate was 1 ml/min. The elution used was gradient mode. The HPLC column used for the analysis was symmetry C18 with a length of 250 mm, the internal diameter of 4.6 mm and particle size of 5.0 microns.Results: The developed method was found to be linear with the range of 0.006-250% with a coefficient of correlation 0.99. The precision study revealed that the percentage relative standard deviation was within the acceptable limit. The limit of detection and limit of quantitation of the impurities was less than 0.002%and 0.006% with respect to pioglitazone hydrochloride test concentration of 2000 µg/ml respectively. This method has been validated as per ICH guidelines Q2 (R1).Conclusion: A reliable, economical HPLC method was magnificently established for quantitative analysis of related substances of pioglitazone hydrochloride drug substance.

scholarly journals Development and validation of reversed phase high performance liquid chromatography (RP-HPLC) for quantification of captopril in rabbit plasma

2020 ◽  
Author(s):  
Muhammad Fawad Rasool ◽  
Umbreen Fatima Qureshi ◽  
Nazar Muhammad Ranjha ◽  
Imran Imran ◽  
Mouqadus Un Nisa ◽  
...  
Keyword(s):  
High Performance Liquid Chromatography ◽  
Liquid Chromatography ◽  
Mobile Phase ◽  
High Performance ◽  
Limit Of Detection ◽  
Reversed Phase ◽  
Rabbit Plasma ◽  
Rp Hplc ◽  
Relative Standard

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.

scholarly journals Coupling multiplex pre-amplification and droplet digital PCR for longitudinal monitoring ofESR1andPIK3CAmutations from plasma cell-free DNA

2019 ◽  
Author(s):  
Huilan Yao ◽  
Grant Wu ◽  
Subhasree Das ◽  
Crystal MacKenzie ◽  
Hua Gao ◽  
...  
Keyword(s):  
Limit Of Detection ◽  
Hot Spot ◽  
Metastatic Breast ◽  
High Sensitivity ◽  
Cost Effective ◽  
Digital Pcr ◽  
Cost Effective Method ◽  
High Prevalence ◽  
High Concordance ◽  
Hotspot Mutations

AbstractHere we report on the development of a sensitive and cost-effective method to longitudinally trackESR1andPIK3CAmutations from cfDNA in patients with metastatic breast cancer (MBC) using a streamlined and de-centralized workflow. Hotspot mutations inESR1have been shown to cause resistance to aromatase inhibitor–based and anti-estrogenic therapies, whilePIK3CAmutations have high prevalence in MBC. As a result, their utility as circulating biomarkers to predict or monitor response in the clinical development of investigational compounds has been the focus of many studies. Six regions inESR1andPIK3CAgenes containing 20 hotspot mutations were pre-amplified, followed by optimized singleplex ddPCR assays to detect allele frequencies of individual mutations. Without pre-amplification, the limit of detection (LOD) and limit of linearity (LOL) of individual ddPCR assays were at 0.05-0.1% and 0.25% level, respectively. With pre-amplification, the LOD and LOL were slightly elevated at 0.1-0.25% and 0.25-0.5% levels, respectively. High concordance was achieved to the BEAMing assay (Sysmex Inostics) for mutation positive assays (r=0.98, P<0.0001). In conclusion, coupling pre-amplification and ddPCR assays allowed us for the detection of up to 20 hot spot mutations inESR1andPIK3CAwith high sensitivity and reproducibility.

Sign in / Sign up

Export Citation Format

Share Document