scholarly journals Gradient HPLC-Diode Array Detector Stability-Indicating Determination of Lidocaine Hydrochloride and Cetylpyridinium Chloride in Two Combined Oral Gel Dosage Forms

2011 ◽  
Vol 94 (2) ◽  
pp. 503-512 ◽  
Author(s):  
Tarek S Belal ◽  
Rasha A Shaalan ◽  
Rim S Haggag
Keyword(s):  
Mobile Phase ◽  
Cetylpyridinium Chloride ◽  
Gradient Elution ◽  
Lidocaine Hydrochloride ◽  
Array Detector ◽  
Diode Array ◽  
Forced Degradation ◽  
Diode Array Detector ◽  
Stability Indicating

Abstract A simple, rapid, and selective HPLC-diode array detector method was developed for the simultaneous determination of lidocaine hydrochloride (LD) and cetylpyridinium chloride (CPC) in two combined pharmaceutical formulations. Effective chromatographic separation was achieved on a Zorbax SB-C8 (4.6 250 mm, 5 m particle size) column with gradient elution using a mobile phase composed of 0.05 M phosphoric acid and acetonitrile. The gradient elution started with 25 (v/v) acetonitrile, ramped up linearly to 85 in 5 min, and then was constant until the end of the run. The mobile phase was pumped at a flow rate of 1.2 mL/min. The multiple wavelength detector was set at 214 and 258 nm, and quantification of the analytes was based on measuring their peak areas. The retention times for LD and CPC were about 3.4 and 7.3 min, respectively. The reliability and analytical performance of the proposed HPLC procedure were statistically validated with respect to linearity, range, precision, accuracy, selectivity, robustness, LOD, and LOQ. Calibration curves were linear in the range of 5200 and 10400 g/mL for LD and CPC, respectively, with correlation coefficients >0.999. The proposed method was proven to be stability-indicating by the resolution of the two analytes from the related substance and potential impurity (2,6-dimethylaniline) as well as from forced-degradation products. The validated HPLC method was extended to the analysis of LD and CPC in two combined oral gel preparations for which the two analytes were successfully resolved from the pharmaceutical adjuvants and quantified with recoveries not less than 97.9.

scholarly journals Determination of Patulin in Apple Juice by Liquid Chromatography

2006 ◽  
Vol 89 (1) ◽  
pp. 139-143 ◽  
Author(s):  
Maria Helena Iha ◽  
Myrna Sabino
Keyword(s):  
Liquid Chromatography ◽  
Standard Deviation ◽  
Mobile Phase ◽  
Apple Juice ◽  
Array Detector ◽  
Diode Array ◽  
Diode Array Detector ◽  
Relative Standard ◽  
Precision Study

Abstract A method was developed and validated in-house for the determination of patulin (PAT), a toxic mold metabolite, in apple juice. The sample was extracted with ethyl acetatehexane and analyzed by liquid chromatography equipped with a C18 column and diode array detector. The mobile phase used for the quantification was waterethanol, at a flow rate of 0.5 mL/min. The method showed a mean recovery of 84.8%, the relative standard deviation obtained in the precision study was <7.7%, the quantification and detection limits were 7 and 3 μg/L, respectively, and the linear range for PAT in apple juice was 2.6650 μg/L. The ruggedness was evaluated by an intralaboratory experiment, in which 5 factors were studied, and only one was found to influence the observed results. The developed method is fast, practical, and simple; the solvents (except hexane) and reagents used were nontoxic. The results of the validation confirmed the efficiency of the method, which is sensitive enough to be used in studies required to quantify PAT in apple juice.

scholarly journals Development and Validation of a Stability Indicating LC Method for the Assay and Related Substances Determination of a Proteasome Inhibitor Bortezomib

2012 ◽  
Vol 2012 ◽  
pp. 1-13 ◽  
Author(s):  
Kasa Srinivasulu ◽  
Mopidevi Narasimha Naidu ◽  
Kadaboina Rajasekhar ◽  
Murki Veerender ◽  
Mulukutla Venkata Suryanarayana
Keyword(s):  
Formic Acid ◽  
Mobile Phase ◽  
Gradient Elution ◽  
Hplc Method ◽  
Forced Degradation ◽  
Balance Study ◽  
Stability Indicating ◽  
Related Substances ◽  
Mass Balance Study

A novel, simple, sensitive, stability indicating HPLC method was developed and validated for quantification of impurities (process related and degradants) and assay determination of bortezomib. Stability indicating power of the method was established by forced degradation experiments and mass balance study. The chromatographic separation was achieved with Waters SymmetryShield RP18 column using gradient elution using the mobile phase-A consists of a mixture of water-acetonitrile-formic acid (715 : 285 : 1, v/v/v) and the mobile phase-B consists a mixture of methanol-water-formic acid (800 : 200 : 1, v/v/v), respectively. The developed method is validated for parameters like precision, accuracy, linearity, LOD, LOQ, and ruggedness. Central composite experimental design (CCD) was applied to check the robustness of the method. The stability tests were also performed on drug substances as per ICH norms.

Analysis of Paclitaxel in Pharmaceutical Injection by Ultra Performance Convergence Chromatography

2014 ◽  
Vol 989-994 ◽  
pp. 1060-1063
Author(s):  
Xiao Gong ◽  
Xiao Bing Huang ◽  
Yong Hua Wei ◽  
Ning Li Qi ◽  
Li Jing Lin ◽  
...  
Keyword(s):  
Mobile Phase ◽  
Gradient Elution ◽  
Array Detector ◽  
Diode Array ◽  
Diode Array Detector ◽  
Linear Gradient ◽  
Good Linearity ◽  
Good Repeatability

A simple and sensitive ultra-performance convergence chromatography system coupled with a diode array detector for analysis of paclitaxel, 10-deacetyl-7-epipaclitaxel and cephalomannine in paclitaxel injection was developed. The analyses were carried out on a Waters Acquity UPC2 BEH 2-EP using the mobile phase of mixture of supercritical CO2 and methanol with a linear gradient elution from 92:8 to 82:18 at 50 °C. The method offers good linearity, higher resolution, and good repeatability. LOD and LOQ were 0.45 and 1.32 ng, respectively.

scholarly journals Quantitative Determination by HPLC-DAD of Icariin, Epimedin A, Epimedin B, and Epimedin C in Epimedium (Berberidaceae) Species Growing in Turkey

2016 ◽  
Vol 11 (11) ◽  
pp. 1934578X1601101 ◽  
Author(s):  
Derya Cicek Polat ◽  
Maksut Coskun
Keyword(s):  
Quantitative Determination ◽  
Flow Rate ◽  
Mobile Phase ◽  
Hplc Method ◽  
Biologically Active ◽  
Array Detector ◽  
Diode Array ◽  
Gradient System ◽  
Diode Array Detector

The genus Epimedium is rich in terms of flavonoids, of which icariin, epimedin A, epimedin B and epimedin C are known especially to be biologically active. Therefore, it is important to quantify these compounds. In this study, a HPLC method coupled with DAD detection was developed and validated for the determination of icariin, epimedin A, epimedin B and epimedin C in Epimedium species growing in Turkey. The chromatographic separation was performed using a gradient system with a mobile phase of 0.1% formic acid (A) and acetonitrile (B) applied at a flow rate of 1 mL/min using a diode array detector. The highest values were, respectively, icariin 0.65%, epimedin A 0.13%, epimedin B 0.11%, epimedin C 0.06%. The highest values were obtained from the materials collected in Uzungol (Trabzon-Turkey).

scholarly journals Analysis of the Mycosporine-Like Amino Acid (MAA) Pattern of the Salt Marsh Red Alga Bostrychia scorpioides

Marine Drugs ◽  
2021 ◽  
Vol 19 (6) ◽  
pp. 321
Author(s):  
Maria Orfanoudaki ◽  
Anja Hartmann ◽  
Julia Mayr ◽  
Félix L. Figueroa ◽  
Julia Vega ◽  
...  
Keyword(s):  
Amino Acids ◽  
High Performance Liquid Chromatography ◽  
High Performance ◽  
Red Alga ◽  
Array Detector ◽  
Diode Array ◽  
Diode Array Detector ◽  
The Past ◽  
Specific Species

This study presents the validation of a high-performance liquid chromatography diode array detector (HPLC-DAD) method for the determination of different mycosporine-like amino acids (MAAs) in the red alga Bostrychia scorpioides. The investigated MAAs, named bostrychines, have only been found in this specific species so far. The developed HPLC-DAD method was successfully applied for the quantification of the major MAAs in Bostrychia scorpioides extracts, collected from four different countries in Europe showing only minor differences between the investigated samples. In the past, several Bostrychia spp. have been reported to include cryptic species, and in some cases such as B. calliptera, B. simpliciuscula, and B. moritziana, the polyphyly was supported by differences in their MAA composition. The uniformity in the MAA composition of the investigated B. scorpioides samples is in agreement with the reported monophyly of this Bostrychia sp.

scholarly journals Stability indicating HPLC-Fluorescence detection method for the simultaneous determination of linagliptin and empagliflozin in their combined pharmaceutical preparation

2021 ◽  
Vol 12 (2) ◽  
pp. 168-178
Author(s):  
Mohamed Rizk ◽  
Ali Kamal Attia ◽  
Heba Yosry Mohamed ◽  
Mona Elshahed
Keyword(s):  
Fluorescence Detection ◽  
Mobile Phase ◽  
Pharmaceutical Preparation ◽  
Pharmaceutical Preparations ◽  
Forced Degradation ◽  
Stability Indicating ◽  
Accuracy And Precision ◽  
Relative Standard ◽  
Significant Difference

A sensitive, accurate, and precise liquid chromatographic method has been developed and validated for the determination of Linagliptin (LNG) and Empagliflozin (EMP) in their combined tablets. Chromatographic separation was carried out on ODS-3 Inertsil® C18 column (150×4.6 mm, 5 µm). The mobile phase A (consisting of 0.30% Triethyl amine buffer (TEA) at pH = 4.5, adjusted using ortho-phosphoric acid); the mobile phase B (consisting of acetonitrile) was pumped through the column whose temperature was maintained at 40 °C, with a flow rate 1.7 mL/min, using gradient elution from 0-3 min A:B (75:25, v:v), then from 3-6 min the ratio changed to be A:B (60:40, v:v). Fluorescence detection (FLD) was performed at 410 nm after excitation at 239 nm. Acceptable linearity, accuracy and precision values of the proposed method were found over the concentration ranges of 0.5-15 µg/mL for LNG and 1.0-30 µg/mL for EMP with correlation coefficients of 0.9997 and 0.9998 in the case of LNG and EMP, respectively. The recoveries and relative standard deviations percentages were found in the following ranges: 98.56-101.85 and 0.53-1.52% for LNG and 98.00-101.95 and 0.31-1.05% for EMP. The detection and quantification limits were 0.15 and 0.45 µg/mL for LNG and 0.22 and 0.67 µg/mL for EMP. The optimized method was validated and proved to be specific, robust, accurate and reliable for the determination of the drugs in pure form or in their combined pharmaceutical preparations. No significant difference was found regarding accuracy and precision upon statistical comparison between the obtained results of the proposed method and those of the reported method. Furthermore, the proposed method is proved to be a stability-indicating assay after exposure of the studied drugs to variable forced degradation parameters, such as acidic, alkaline and oxidative conditions, according to the recommendations of the International Conference on Harmonization guidelines. The simplicity and selectivity of the proposed method allows its use in quality control laboratories.

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