Automated Fourier Transform near Infrared Determination of Buprofezin in Pesticide Formulations

2005 ◽  
Vol 13 (3) ◽  
pp. 161-168 ◽  
Author(s):  
Sergio Armenta ◽  
Javier Moros ◽  
Salvador Garrigues ◽  
Miguel de la Guardia
Keyword(s):  
Fourier Transform ◽  
High Performance ◽  
Near Infrared ◽  
Limit Of Detection ◽  
Spectroscopic Method ◽  
Sample Treatment ◽  
Pesticide Formulations ◽  
Relative Standard ◽  
On Line

An automated procedure has been developed for Fourier transform near infrared (FT-NIR) determination of buprofezin in pesticide formulations. This methodology is based on on-line pesticide extraction with acetonitrile from solid samples and its determination by using peak area absorbance measurements between 2147 and 2132 nm, corrected with a horizontal baseline established at 2091 nm. The repeatability, as a relative standard deviation of five independent analyses of 18.9 mg g−1 of buprofezin, was 0.06% and the limit of detection 5 mg L−1. The reagent consumption was clearly reduced compared with a chromatographic reference procedure from 40.4 mL acetonitrile per sample, required by high performance liquid chromatography (HPLC), to 2 mL acetonitrile consumed for FT-NIR. The sample measurement throughput obtained by the FT-NIR methodology was 30 h−1, five times higher than that obtained by HPLC (6 h−1). It can be concluded that the proposed vibrational spectroscopic method is appropriate for the quality control of commercial pesticide formulations. The on-line sample treatment avoids contact by the operator with toxic products and this method is an environmentally friendly alternative to the measurement in the mid infrared which requires the use of CHCl3.

scholarly journals A Comparative Study of First-Derivative Spectrophotometry and Column High-Performance Liquid Chromatography Applied to the Determination of Repaglinide in Tablets and for Dissolution Testing

2008 ◽  
Vol 91 (3) ◽  
pp. 530-535 ◽  
Author(s):  
Bashar A AlKhalidi ◽  
Majed Shtaiwi ◽  
Hatim S AlKhatib ◽  
Mohammad Mohammad ◽  
Yasser Bustanji
Keyword(s):  
High Performance ◽  
Limit Of Detection ◽  
Spectroscopic Method ◽  
High Performance Liquid Chromatographic ◽  
Dissolution Testing ◽  
First Derivative ◽  
Relative Standard ◽  
Limit Of Quantitation ◽  
Significant Difference

Abstract A fast and reliable method for the determination of repaglinide is highly desirable to support formulation screening and quality control. A first-derivative UV spectroscopic method was developed for the determination of repaglinide in tablet dosage form and for dissolution testing. First-derivative UV absorbance was measured at 253 nm. The developed method was validated for linearity, accuracy, precision, limit of detection (LOD), and limit of quantitation (LOQ) in comparison to the U.S. Pharmacopeia (USP) column high-performance liquid chromatographic (HPLC) method. The first-derivative UV spectrophotometric method showed excellent linearity [correlation coefficient (r) = 0.9999] in the concentration range of 135 g/mL and precision (relative standard deviation <1.5). The LOD and LOQ were 0.23 and 0.72 g/mL, respectively, and good recoveries were achieved (98101.8). Statistical comparison of results of the first-derivative UV spectrophotometric and the USP HPLC methods using the t-test showed that there was no significant difference between the 2 methods. Additionally, the method was successfully used for the dissolution test of repaglinide and was found to be reliable, simple, fast, and inexpensive.

scholarly journals Salting-Out Induced Liquid-Liquid Microextraction for Alogliptin Benzoate Determination in Human Plasma by HPLC/UV

2020 ◽  
Author(s):  
Sherin Farouk Hammad ◽  
Inas Abdallah ◽  
Alaa Bedair ◽  
Fotouh Mansour
Keyword(s):  
High Performance ◽  
Limit Of Detection ◽  
Hplc Method ◽  
Aqueous Sample ◽  
Sample Treatment ◽  
Salting Out ◽  
Relative Standard ◽  
Limit Of Quantitation ◽  
Liquid Microextraction

Abstract Salting-out induced liquid-liquid microextraction method has been developed for plasma sample treatment before determination of alogliptin by high performance liquid chromatography with UV detection. Several parameters were optimized to achieve maximum enrichment, including type of extractant, volume of extractant, type of anion, type of cation, salt amount and pH. The optimum conditions were attained using 500 µL of acetonitrile, added to 1 mL of aqueous sample containing 250 mg of sodium chloride at pH 12. An RP-HPLC method was developed and validated according to the International Conference on Harmonization guidelines M10. The method was linear in the concentration range of 0.1 to 50 µg/mL (correlation coefficient= 0.997). The limit of detection was 19 ng/mL and limit of quantitation was 60 ng /mL. The method was accurate and precise with an average % recovery of 99.7% and a % relative standard deviation ranging between 1.5 and 2.5. These results showed that the salting-out induced liquid-liquid microextraction methods could be better than other sample preparation protocols in terms of sensitivity, easiness, solvent consumption and waste reduction.

scholarly journals Salting-Out Induced Liquid-Liquid Microextraction for Alogliptin Benzoate Determination in Human Plasma by HPLC/UV

2020 ◽  
Author(s):  
Sherin Farouk Hammad ◽  
Inas Abdallah ◽  
Alaa Bedair ◽  
Fotouh Mansour
Keyword(s):  
High Performance ◽  
Limit Of Detection ◽  
Hplc Method ◽  
Aqueous Sample ◽  
Sample Treatment ◽  
Salting Out ◽  
Relative Standard ◽  
Limit Of Quantitation ◽  
Liquid Microextraction

Abstract Salting-out induced liquid-liquid microextraction method has been developed for plasma sample treatment before determination of alogliptin by high performance liquid chromatography with UV detection. Several parameters were optimized to achieve maximum enrichment, including type of extractant, volume of extractant, type of anion, type of cation, salt amount and pH. The optimum conditions were attained using 500 µL of acetonitrile, added to 1 mL of aqueous sample containing 250 mg of sodium chloride at pH 12. An RP-HPLC method was developed and validated according to the International Conference on Harmonization guidelines M10. The method was linear in the concentration range of 0.1 to 50 µg/mL (correlation coefficient= 0.997). The limit of detection was 0.019 µg/mL and limit of quantitation was 0.06 µg/mL. The method was accurate and precise with an average % recovery of 99.7% and a % relative standard deviation ranging between 1.5 and 2.5. These results showed that the salting-out induced liquid-liquid microextraction methods could be better than other sample preparation protocols in terms of sensitivity, easiness, solvent consumption and waste reduction.

scholarly journals Salting-out induced liquid–liquid microextraction for alogliptin benzoate determination in human plasma by HPLC/UV

BMC Chemistry ◽  
2021 ◽  
Vol 15 (1) ◽  
Author(s):  
Sherin F. Hammad ◽  
Inas A. Abdallah ◽  
Alaa Bedair ◽  
Fotouh R. Mansour
Keyword(s):  
High Performance ◽  
Limit Of Detection ◽  
Hplc Method ◽  
Aqueous Sample ◽  
Sample Treatment ◽  
Salting Out ◽  
Relative Standard ◽  
Limit Of Quantitation ◽  
Liquid Microextraction

AbstractSalting-out induced liquid–liquid microextraction method has been developed for plasma sample treatment before determination of alogliptin by high performance liquid chromatography with UV detection. Several parameters were optimized to achieve maximum enrichment, including type of extractant, volume of extractant, type of anion, type of cation, salt amount and pH. The optimum conditions were attained using 500 µL of acetonitrile, added to 1 mL of aqueous sample containing 250 mg of sodium chloride at pH 12. An RP-HPLC method was developed and validated according to the International Conference on Harmonization guidelines M10. The method was linear in the concentration range of 0.1 to 50 µg/mL (correlation coefficient = 0.997). The limit of detection was 0.019 µg/mL and limit of quantitation was 0.06 µg/mL. The method was accurate and precise with an average % recovery of 99.7% and a % relative standard deviation ranging between 1.5 and 2.5. These results showed that the salting-out induced liquid–liquid microextraction methods could be better than other sample preparation protocols in terms of sensitivity, easiness, solvent consumption and waste reduction.

scholarly journals Salting-Out Induced Liquid-Liquid Microextraction for Alogliptin Benzoate Determination in Human Plasma by HPLC/UV

2020 ◽  
Author(s):  
Sherin Farouk Hammad ◽  
Inas Abdallah ◽  
Alaa Bedair ◽  
Fotouh Mansour
Keyword(s):  
High Performance ◽  
Limit Of Detection ◽  
Hplc Method ◽  
Aqueous Sample ◽  
Sample Treatment ◽  
Salting Out ◽  
Relative Standard ◽  
Limit Of Quantitation ◽  
Liquid Microextraction

Abstract Salting-out induced liquid-liquid microextraction method has been developed for plasma sample treatment before determination of alogliptin by high performance liquid chromatography with UV detection. Several parameters were optimized to achieve maximum enrichment, including type of extractant, volume of extractant, type of anion, type of cation, salt amount and pH. The optimum conditions were attained using 500 µL of acetonitrile, added to 1 mL of aqueous sample containing 250 mg of sodium chloride at pH 12. An RP-HPLC method was developed and validated according to the International Conference on Harmonization guidelines M10. The method was linear in the concentration range of 0.1 to 50 µg /mL (correlation coefficient= 0.997). The limit of detection was 0.019 µg/mL and limit of quantitation was 0.06 µ g/mL. The method was accurate and precise with an average % recovery of 99.7% and a % relative standard deviation ranging between 1.5 and 2.5. These results showed that the salting-out induced liquid-liquid microextraction methods could be better than other sample preparation protocols in terms of sensitivity, easiness, solvent consumption and waste reduction.

scholarly journals Salting-Out Induced Liquid-Liquid Microextraction for Alogliptin Benzoate Determination in Human Plasma by HPLC/UV

2020 ◽  
Author(s):  
Sherin Farouk Hammad ◽  
Inas Abdallah ◽  
Alaa Bedair ◽  
Fotouh Mansour
Keyword(s):  
High Performance ◽  
Limit Of Detection ◽  
Hplc Method ◽  
Aqueous Sample ◽  
Sample Treatment ◽  
Salting Out ◽  
Relative Standard ◽  
Limit Of Quantitation ◽  
Liquid Microextraction

Abstract Salting-out induced liquid-liquid microextraction method has been developed for plasma sample treatment before determination of alogliptin by high performance liquid chromatography with UV detection. Several parameters were optimized to achieve maximum enrichment including type of extractant, volume of extractant, type of anion, type of cation, salt amount and pH. The optimum conditions were achieved using 500 µL of acetonitrile, added to 1 mL of aqueous sample containing 250 mg of sodium chloride at pH 12. An RP-HPLC method was developed and validated according to the International Conference on Harmonization guidelines Q2 (R1). The method was linear in the concentration range of 0.1 to 50 µg/mL (correlation coefficient= 0.997). The limit of detection was 19 ng/mL and limit of quantitation was 60 ng /mL. The method was accurate and precise with a % recovery of 99.7% and a % relative standard deviation ranging between 1.5 and 2.5. These results showed that the salting-out induced liquid-liquid microextraction methods could be better than other sample preparation protocols in terms of sensitivity, easiness, solvent consumption and waste reduction.

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 Determination of Tianeptine in Tablets by High-Performance Liquid Chromatography with Fluorescence Detection

2007 ◽  
Vol 90 (3) ◽  
pp. 720-724
Author(s):  
Sevgi Tatar Ulu
Keyword(s):  
Lower Limit ◽  
High Performance ◽  
Limit Of Detection ◽  
Internal Standard ◽  
Linear Calibration ◽  
Fluorescence Detector ◽  
Relative Standard ◽  
Validation Parameters ◽  
Limit Of Quantitation

Abstract A sensitive and selective high-performance liquid chromatographic method has been developed for the determination of tianeptine (Tia) in tablets. The method is based on derivatization of Tia with 4-chloro-7-nitrobenzofurazan (NBD-Cl). A mobile phase consisting of acetonitrile10 mM orthophosphoric acid (pH 2.5; 77 + 23) was used at a flow rate of 1 mL/min on a C18 column. The Tia-NBD derivative was monitored using a fluorescence detector, with emission set at 520 nm and excitation at 458 nm. Gabapentin was selected as an internal standard. Linear calibration graphs were obtained in the concentration range of 45300 ng/mL. The lower limit of detection (LOD) was 10 ng/mL at a signal-to-noise ratio of 4. The lower limit of quantitation (LOQ) was 45 ng/mL. The relative standard values for intra- and interday precision were <0.46 and <0.57%, respectively. The recovery of the drug samples ranged between 98.89 and 99.85%. No chromatographic interference from the tablet excipients was found. The proposed method was validated in terms of precision, robustness, recovery, LOD, and LOQ. All the validation parameters were within the acceptance range. The proposed method was applied for the determination of Tia in commercially available tablets. The results were compared with those obtained by an ultraviolet spectrophotometric method using t- and F-tests.

scholarly journals Quantitative Determination of Triterpenes from Amphiptherygium adstringens by Liquid Chromatography and Thin-Layer Chromatography and Morphological Analysis of Cuachalalate Preparations

2006 ◽  
Vol 89 (1) ◽  
pp. 1-7 ◽  
Author(s):  
Andrés Navarrete ◽  
Bharathi Avula ◽  
Vaishali C Joshi ◽  
Xiuhong Ji ◽  
Paul Hersh ◽  
...  
Keyword(s):  
Thin Layer ◽  
Thin Layer Chromatography ◽  
High Performance ◽  
Limit Of Detection ◽  
Gastric Ulcers ◽  
Array Detector ◽  
Plant Materials ◽  
Relative Standard ◽  
Layer Chromatography

Abstract Amphiptherygium adstringens (Anacardiaceae/Julianaceae), local name cuachalalate, is used in folk medicine for the treatment of cholelithiasis, fevers, fresh wounds, hypercholesterolemia, gastritis, gastric ulcers, and cancer of the gastrointestinal tract. The development of column high-performance liquid chromatographyphotodiode array detector (LC-PDA) and high-performance thin-layer chromatography (HPTLC)densitometry methods for the determination of masticadienonic acid and 3-hydroxymasticadienonic acid in cuachalalate preparations is described in this paper. Good separation of the compounds could be achieved by both methods. Either might be preparable depending on the requirements. The LC separation was performed on a Phenomenex Synergi MAX-RP 80A reversed-phase column operated at 40C with detection at 215 nm. The plant materials were extracted with methanol by sonication. The triterpenes present in the plant material and commercial extracts were separated with an acetonitrilewater reagent alcohol isocratic system. The limit of detection was 0.10.2 g/mL. The relative standard deviation values for the determination of triterpenes in plant extracts were less than 1.00%. This is the first report of an analytical method developed for the quantitative analysis of triterpenes from Amphiptherygium adstringens by LC-PDA and HPTLC. The stem bark showed higher amounts of triterpenes, and low amounts in root and stem root. The microscopic description of the crude drug of cuachalalate was also provided.

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