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 ◽  
...  

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.

2021 ◽  
Vol 7 (1) ◽  
Author(s):  
Hina Shamshad ◽  
Agha Zeeshan Mirza

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.


2013 ◽  
Vol 781-784 ◽  
pp. 787-791 ◽  
Author(s):  
Ya Li Xing ◽  
Liang Wu Bi ◽  
Zhen Dong Zhao ◽  
Tian Juan Xia

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.


2011 ◽  
Vol 94 (1) ◽  
pp. 106-109 ◽  
Author(s):  
Suryakant D Bhosale ◽  
Sadhana J Rajput

Abstract An RP-HPLC method has been developed for the simultaneous determination of butenafine hydrochloride and betamethasone dipropionate on an Inertsil C18 column (250×4.6 mm id) using a mobile phase gradient consisting of methanol and water at a flow rate of 1 mL/min. Detection was carried out at 254 nm. Retention times of betamethasone dipropionate and butenafine hydrochloride were 4.82 (±0.80) and 16.18 (±0.17) min, respectively. The method was validated with respect to specificity, linearity, accuracy, precision, ruggedness, and robustness. This method is simple, precise, and sensitive, and applicable for the simultaneous quantification of butenafine hydrochloride and betamethasone dipropionate in a cream formulation.


Separations ◽  
2021 ◽  
Vol 8 (1) ◽  
pp. 5
Author(s):  
Mohd Afzal ◽  
Mohd. Muddassir ◽  
Abdullah Alarifi ◽  
Mohammed Tahir Ansari

A highly specific, accurate, and simple RP-HPLC technique was developed for the real-time quantification of domperidone (DOMP) and lansoprazole (LANS) in commercial formulations. Chromatographic studies were performed using a Luna C8(2), 5 μm, 100Å, column (250 × 4.6 mm, Phenomenex) with a mobile phase composed of acetonitrile/2 mM ammonium acetate (51:49 v/v), pH 6.7. The flow rate was 1 mL·min−1 with UV detection at 289 nm. Linearity was observed within the range of 4–36 µg·mL−1 for domperidone and 2–18 µg·mL−1 for lansoprazole. Method optimization was achieved using Box-Behnken design software, in which three key variables were examined, namely, the flow rate (A), the composition of the mobile phase (B), and the pH (C). The retention time (Y1 and Y3) and the peak area (Y2 and Y4) were taken as the response parameters. We observed that slight alterations in the mobile phase and the flow rate influenced the outcome, whereas the pH exerted no effect. Method validation featured various ICH parameters including linearity, limit of detection (LOD), accuracy, precision, ruggedness, robustness, stability, and system suitability. This method is potentially useful for the analysis of commercial formulations and laboratory preparations.


2006 ◽  
Vol 3 (1) ◽  
pp. 60-64 ◽  
Author(s):  
P. Venkata Reddy ◽  
B. Sudha Rani ◽  
G. Srinu Babu ◽  
J. V. L. N. Seshagiri Rao

A reverse phase HPLC method is developed for the determination of Raloxifene in pharmaceutical dosage forms. Chromatography was carried out on an inertsil C18 column using a mixture of acetonitrile and phosphate buffer (30:70 v/v) as the mobile phase at a flow rate of 1 mL/min. Detection was carried out at 290 nm .The retention time of the drug was 10.609 min. The method produced linear responses in the concentration range of 0.5-200 µg/mL of Raloxifene. The method was found to be applicable for determination of the drug in tablets.


2011 ◽  
Vol 94 (2) ◽  
pp. 523-530 ◽  
Author(s):  
Sakshi Gupta ◽  
Gulshan Bansal

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.


2013 ◽  
Vol 96 (1) ◽  
pp. 56-59 ◽  
Author(s):  
Agha Zeeshan Mirza ◽  
M Saeed Arayne ◽  
Najma Sultana

Abstract The objective of this research was to develop and validate a rapid, economical, and sensitive HPLC method for quantitative determination of gliquidone, pioglitazone hydrochloride, and atorvastatin in tablets and serum. Due to drug combination of these formulations, there has been a need for a reliable quantitative method to determine these drugs in commercial samples and human serum. The chromatographic separation was carried out at ambient temperature with a mobile phase consisting of methanol–water (90 + 10, v/v), with pH adjusted to 3.50 with phosphoric acid. The pump was operated at a flow rate of 1 mL/min, and all analytes were detected at 235 nm. The method was linear over the concentration range of 5–50 μg/mL for all the drugs. The LOD of gliquidone, pioglitazone hydrochloride, and atorvastatin was 0.30, 1.30, and 0.57 μg/mL and LOQ was 0.98, 4.28, and 1.90 μg/mL, respectively. The proposed method was successfully applied to the determination of these drugs in commercial tablets and human serum. The established method was validated with respect to specificity, linearity, precision, accuracy, and ruggedness.


2016 ◽  
Vol 2016 ◽  
pp. 1-8 ◽  
Author(s):  
Bürge Aşçı ◽  
Şule Dinç Zor ◽  
Özlem Aksu Dönmez

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.


2012 ◽  
Vol 581-582 ◽  
pp. 68-72
Author(s):  
Chu Qin Yu ◽  
Hua Qing Lin ◽  
Yue Han Hou ◽  
Zhong Feng Shi ◽  
Di Shi Lin

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.


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