scholarly journals QuEChERS-HPLC-DAD method for sulphonamides in chicken breast

2013 ◽  
Vol 49 (1) ◽  
pp. 155-166 ◽  
Author(s):  
Simone Caetani Machado ◽  
Mariane Landin-Silva ◽  
Patrícia Penido Maia ◽  
Susanne Rath ◽  
Isarita Martins
Keyword(s):  
Food Safety ◽  
Simultaneous Determination ◽  
Flow Rate ◽  
Mobile Phase ◽  
Chicken Breast ◽  
Quechers Method ◽  
Initial Flow ◽  
The Matrix ◽  
Interday Precision

The development of a QuEChERS-HPLC-DAD method using a Lichrospher 60 RP-Select B column (250 x 4.6 mm x 5 µm) at 40ºC, mobile phase constituted by phosphate buffer:acetonitrile (75:25, v/v) at a initial flow rate of 0.5 mL min-1, increased by 1.2 mL min-1 and at 265 nm is presented for simultaneous determination of sulphadiazine, sulphametoxipiridazine and sulphamethoxazole in chicken breast samples. QuEchERS is inexpensive, fast and easy, and the extraction of the analytes of the matrix was successfully employed. In addition, the method presented linearity, in the range of 25, 50, 100, 150, 175, and 200 µg kg-1, precision, selectivity and sensitivity. The intraday precision (RSD %) for QuEChERS method was between 3.6-10.8 (SDZ), 6.9-14.1 (SPZ) and 1.9-10.9 (SMX) and interday precision (RSD%) was between 1.5-9.7, 1.7-4.1 and 2.1-10.2, respectively. Results of accuracy (bias) were in the range of -8.6 to +11.9 %. Therefore, the validated method is clearly useful for the practical residue monitoring of the drugs evaluated in chicken samples, as all the values were within the acceptable criteria used for food safety. Of 6 samples analyzed, none of them showed contamination of the sulphonamides studied at detectable levels.

scholarly journals Validated Stability-Indicating HPLC-UV Method for Simultaneous Determination of Glipizide and Four Impurities

2011 ◽  
Vol 94 (2) ◽  
pp. 523-530 ◽  
Author(s):  
Sakshi Gupta ◽  
Gulshan Bansal
Keyword(s):  
Simultaneous Determination ◽  
Flow Rate ◽  
Retention Time ◽  
Mobile Phase ◽  
Stability Testing ◽  
Stability Indicating ◽  
Chromatographic Parameters ◽  
Interday Precision ◽  
Calculated Amount

Abstract A selective stability-indicating HPLC-UV method for simultaneous determination of glipizide and four impurities (DPs IIV) formed under hydrolytic conditions was developed and validated. The drug and impurities were resolved on an XTerra C18 column (250 4.5 mm id) in a single gradient run using buffer (0.005 M KH2PO4; pH 3.0)methanol (60 40, v/v; mobile phase A) and (20 80, v/v; mobile phase B) at a flow rate of 0.5 mL/min with 230 nm detection wavelength. The method was linear across concentration ranges of 0.2100, 0.1100, 0.5100, 0.2100, and 0.150 0000g/mL for glipizide and DPs IIV, respectively. The RSD for intraday and interday precision for the drug and impurities was <1 and <1.2, respectively. Satisfactory recoveries (96.5899.97) of each of the three concentrations selected across the linearity range of each analyte were obtained, proving the method was sufficiently accurate. The LOD was 0.07, 0.05, 0.16, 0.08, and 0.05 g/mL and the LOQ was 0.20, 0.14, 0.50, 0.23, and 0.14 g/mL for the drug and DPs IIV, respectively. Each peak was resolved with resolution of >2 from the nearest peak. Insignificant changes in retention time (<4) and calculated amount (<1.65) of drug and each impurity upon small but deliberate changes in various chromatographic parameters were observed, suggesting the method was robust. The method was applied successfully to stability testing of glipizide tablets.

scholarly journals Development and Validation of HPLC Method for the Simultaneous Determination of Five Food Additives and Caffeine in Soft Drinks

2016 ◽  
Vol 2016 ◽  
pp. 1-8 ◽  
Author(s):  
Bürge Aşçı ◽  
Şule Dinç Zor ◽  
Özlem Aksu Dönmez
Keyword(s):  
Simultaneous Determination ◽  
Flow Rate ◽  
Mobile Phase ◽  
High Performance ◽  
Food Additives ◽  
Hplc Method ◽  
Soft Drinks ◽  
Phase Ratio ◽  
Potassium Sorbate

Box-Behnken design was applied to optimize high performance liquid chromatography (HPLC) conditions for the simultaneous determination of potassium sorbate, sodium benzoate, carmoisine, allura red, ponceau 4R, and caffeine in commercial soft drinks. The experimental variables chosen were pH (6.0–7.0), flow rate (1.0–1.4 mL/min), and mobile phase ratio (85–95% acetate buffer). Resolution values of all peak pairs were used as a response. Stationary phase was Inertsil OctaDecylSilane- (ODS-) 3V reverse phase column (250 × 4.6 mm, 5 μm) dimensions. The detection was performed at 230 nm. Optimal values were found 6.0 pH, 1.0 mL/min flow rate, and 95% mobile phase ratio for the method which was validated by calculating the linearity (r2>0.9962), accuracy (recoveries ≥ 95.75%), precision (intraday variation ≤ 1.923%, interday variation ≤ 1.950%), limits of detection (LODs), and limits of quantification (LOQs) parameters. LODs and LOQs for analytes were in the range of 0.10–0.19 μg/mL and 0.33–0.63 μg/mL, respectively. The proposed method was applied successfully for the simultaneous determination of the mixtures of five food additives and caffeine in soft drinks.

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.

scholarly journals Simultaneous Determination of Four Active Ingredients inSargentodoxa cuneataby HPLC Coupled with Evaporative Light Scattering Detection

2016 ◽  
Vol 2016 ◽  
pp. 1-7 ◽  
Author(s):  
Di-Hua Li ◽  
Yuan-Shan Lv ◽  
Jun-Hong Liu ◽  
Lei Yang ◽  
Yan Wang ◽  
...  
Keyword(s):  
Light Scattering ◽  
Simultaneous Determination ◽  
Flow Rate ◽  
Evaporative Light Scattering Detection ◽  
Light Scattering Detection ◽  
Evaporative Light Scattering ◽  
Relative Standard ◽  
Acid Aqueous Solution ◽  
Interday Precision

A HPLC coupled with evaporative light scattering detection method had been developed for the simultaneous determination of 3,4-dihydroxyphenylethyl alcohol glycoside, salidroside, chlorogenic acid, and liriodendrin in the stem ofSargentodoxa cuneata. With a C18 column, the analysis was performed using acetonitrile and 0.2% formic acid aqueous solution as mobile phase in gradient program at a flow rate of 0.9 mL/min. The optimum drift tube temperature of evaporative light scattering detection was at 105°C with the air flow rate of 2.5 L/min. The calibration curves showed good linearity during the test ranges. This method was validated for limits of detection and quantification, precision, and reproducibility. The recoveries were within the range of 96.39%–104.64%. The relative standard deviations of intraday and interday precision were less than 2.90% and 3.30%, respectively. The developed method can be successfully used to quantify the four analytes in the stem ofSargentodoxa cuneatafrom various regions in China.

scholarly journals A Validated HPLC-DAD Method for Simultaneous Determination of Etodolac and Pantoprazole in Rat Plasma

2014 ◽  
Vol 2014 ◽  
pp. 1-8 ◽  
Author(s):  
Ali S. Abdelhameed ◽  
Samar A. Afifi
Keyword(s):  
Simultaneous Determination ◽  
Mobile Phase ◽  
Rat Plasma ◽  
Array Detector ◽  
Therapeutic Drug ◽  
Ich Guidelines ◽  
Photodiode Array Detector ◽  
Photodiode Array ◽  
Interday Precision

A simple, sensitive, and accurate HPLC-DAD method has been developed and validated for the simultaneous determination of pantoprazole and etodolac in rat plasma as a tool for therapeutic drug monitoring. Optimal chromatographic separation of the analytes was achieved on a Waters Symmetry C18 column using a mobile phase that consisted of phosphate buffer pH~4.0 as eluent A and acetonitrile as eluent B in a ratio of A : B, 55 : 45 v/v for 6 min, pumped isocratically at a flow rate of 0.8 mL min−1. The eluted analytes were monitored using photodiode array detector set to quantify samples at 254 nm. The method was linear withr2=0.9999for PTZ andr2=0.9995for ETD at a concentration range of 0.1–15 and 5–50 μgmL−1for PTZ and ETD, respectively. The limits of detection were found to be 0.033 and 0.918 μgmL−1for PTZ and ETD, respectively. The method was statistically validated for linearity, accuracy, precision, and selectivity following the International Conference for Harmonization (ICH) guidelines. The reproducibility of the method was reliable with the intra- and interday precision (% RSD) <7.76% for PTZ and <7.58 % for ETD.

scholarly journals Application of RP-HPLC method for the simultaneous determination of cetirizine in the presence of quinolones

2021 ◽  
Vol 7 (1) ◽  
Author(s):  
Hina Shamshad ◽  
Agha Zeeshan Mirza
Keyword(s):  
Human Serum ◽  
Simultaneous Determination ◽  
Flow Rate ◽  
Mobile Phase ◽  
Diclofenac Sodium ◽  
Internal Standard ◽  
Hplc Method ◽  
Rp Hplc ◽  
Ich Guidelines

Abstract Background Present work describes a fast, simple, and sensitive procedure for the simultaneous determination of cetirizine in the presence of quinolones using diclofenac sodium as an internal standard. The present work was designed to analyze these compounds in pharmaceutical and clinical labs being economical for use. Results The mobile phase consisted of the simple composition of methanol, acetonitrile, and water in a ratio of 50:20:30 with a pH adjusted to 3.1 at a flow rate of 1 mL min−1. The UV detection was performed at 225 nm. The linearity was assessed over the range of 2.5–50 μg mL−1 for all drugs. The parameters such as accuracy, precision, linearity (>0.999), and sensitivity were satisfactory. Conclusion The method was equally applicable for formulation and human serum with recovery values between 95 and 105%. The results of the method were validated statistically according to ICH guidelines.

scholarly journals BIOANALYTICAL METHOD BY COLUMN-SWITCHING WITH DIRECT INJECTION OF HUMAN PLASMA FOR DETERMINATION OF SULPHONYLUREAS

2019 ◽  
Vol 3 (1) ◽  
pp. 16-22
Author(s):  
Juliana Veloso Ferreira ◽  
Gerson A. Pianetti ◽  
Christian Fernandes
Keyword(s):  
Simultaneous Determination ◽  
Human Plasma ◽  
Flow Rate ◽  
Mobile Phase ◽  
Direct Injection ◽  
Column Switching ◽  
Chromatographic System ◽  
Bioanalytical Method ◽  
Core Column

Sulphonylureas are widely used in the treatment of Diabetes mellitus, one of the main causes of death in human population. Their determination is essential in pharmacological research and in the development of new drugs. Generally, determination of sulphonylureas in biological matrices is performed using conventional sample preparation techniques, which frequently leads to an increase of analysis time and errors. In this context, a bioanalytical method for the simultaneous determination of sulphonylureas by direct injection of human plasma was developed and optimized. An automated column-switching high performance liquid chromatographic system with a restricted access media (RAM) column coupled to a fused-core column was employed. At the first dimension, a RAM column with mobile phase of ultrapure water pH 6.0 at a flow-rate of 1.0 mL min-1 was used. The valve switching time was 3 minutes. At the second dimension, a C18 guard-column coupled to a C18 fused core column with mobile phase of acetonitrile and 10 mM phosphate buffer pH 3.0 (54:46 v/v) at a flow-rate of 0.8 mL min-1 were employed. The column switching system was performed in backflush configuration with an analyte elution time of 1 minute. Flufenamic acid was used as the internal standard. The mean plasma protein exclusion percentage by the RAM-column was 104.5%. The developed and optimized method showed to be fast and simple, allowing the direct injection of biological sample into the chromatographic system and the simultaneous determination of three sulphonylureas in only 12 minutes, including the sample treatment, separation and detection.

scholarly journals Simultaneous Determination of Florfenicol and Diclazuril in Compound Powder by RP-HPLC-UV Method

2014 ◽  
Vol 2014 ◽  
pp. 1-5 ◽  
Author(s):  
Leilei Guo ◽  
Xiangqin Tian ◽  
Shangran Shan ◽  
Jian Han ◽  
Xiaojun Shang ◽  
...  
Keyword(s):  
Phosphoric Acid ◽  
Simultaneous Determination ◽  
Flow Rate ◽  
Mobile Phase ◽  
Analytical Column ◽  
International Conference ◽  
Compound Powder ◽  
Rp Hplc ◽  
Calibration Curves

A RP-HPLC-UV method was developed and validated for simultaneous determination of florfenicol and diclazuril in compound powder. The separation involved using a SinoChoom ODS-BP C18(5 μm, 4.6 mm × 250 mm) analytical column. The mobile phase was a mixture of acetonitrile-0.2% phosphoric acid (pH was adjusted to 3.0 with triethylamine). The ratio of acetonitrile and 0.2% phosphoric acid in the mobile phase was 60 : 40 (v/v) from 0 minutes to 6 minutes and 70 : 30 (v/v) from 6.1 minutes to 15 minutes. The flow rate was 1 mL/min. The temperature of the analytical column was maintained at 30°C. The detection was monitored at 225 nm and 277 nm for florfenicol and diclazuril, respectively. The excipients in the compound powder did not interfere with the drug peaks. The calibration curves of florfenicol and diclazuril were fairly linear over the concentration ranges between 50.0–500.0 μg/mL (r=0.9995) and 10.0–100.0 μg/mL (r=0.9992), respectively. The RSD of both the intraday and interday variations was below 2.1% for florfenicol and diclazuril. The method was successfully validated according to International Conference on Harmonisation and proved to be suitable for the simultaneous determination of florfenicol and diclazuril in compound powder.

Simultaneous Determination of Oleanolic Acid and Ursolic Acid in Leaves of Paulownia by HPLC

2013 ◽  
Vol 781-784 ◽  
pp. 787-791 ◽  
Author(s):  
Ya Li Xing ◽  
Liang Wu Bi ◽  
Zhen Dong Zhao ◽  
Tian Juan Xia
Keyword(s):  
Phosphoric Acid ◽  
Simultaneous Determination ◽  
Ursolic Acid ◽  
Oleanolic Acid ◽  
Flow Rate ◽  
Mobile Phase ◽  
Leaf Extract ◽  
Hplc Method ◽  
Simultaneous Quantification

A quick and accurate HPLC method has been developed for the simultaneous quantification of two bioactive triterpenes, ursolic acid and oleanolic acid in Paulownia leaves. The samples were analyzed on a Shim-pack ODS-CLC (M) (4.6 mm × 250 mm, 5 μm) column kept at 21 °C, using the methanol and aqueous phase containing 0.05%phosphoric acid with the volumetric ratio of 91.7:8.3 as the mobile phase at a flow rate of 0.6 mL/ min, and the detection wavelength was set at 210 nm. The method was validated and applied to the simultaneous quantification of the two triterpenes in Paulownia leaf extract. The standard curves were established in the range of 0.44 ~ 8.75 μg for oleanolic acid and 0.92 ~ 18.37 μg for ursolic acid. The contents of oleanolic acid and ursolic acid in leaves of Paulownia were determinated using the HPLC method and the contents were 3.87 mg/g and 13.61 mg/g, respectively.

scholarly journals A Simple and Convenient Method for Simultaneous Determination ofSchizandrol A,Schizandrol B,Schisandrin A,γ-Schisandrin, andSchisandrin C

2016 ◽  
Vol 2016 ◽  
pp. 1-7 ◽  
Author(s):  
Yu Zhou ◽  
Wu Ling Wei ◽  
Jiang Xing Hua ◽  
Qingsheng Fan
Keyword(s):  
Simultaneous Determination ◽  
Flow Rate ◽  
Convenient Method ◽  
Mobile Phase ◽  
Gradient Elution ◽  
Hplc Method ◽  
Schisandra Chinensis ◽  
Column Temperature

A simple, rapid, and specific HPLC method was established for simultaneous determination of five major lignans (Schizandrol A,Schizandrol B,Schisandrin A,γ-Schisandrin, andSchisandrin C) inSchisandra chinensis. The five lignans can be separated completely on Kromasil C18column (250 nm × 4.6 nm) and then detected at 254 nm using methanol (mobile phase A) and water (mobile phase B) with gradient elution as the mobile phase at 1.0 mL/min flow rate. The column temperature was 30°C. The method was validated in terms of linearity, precision, stability, repeatability, and recovery. Results showed that the method is accurate and reproducible.

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