Determination of Chloramphenicol, Thiamphenicol and Florfenicol in Chinese Gelatin Medicines using Dispersive Solid-Phase Extraction Coupled with Ultra High-Performance Liquid Chromatography-Mass Spectrometry.

2020 ◽  
Vol 58 (5) ◽  
pp. 471-476 ◽  
Author(s):  
Jiong Li ◽  
Jinyan Gong ◽  
Haina Yuan ◽  
Gongnian Xiao ◽  
Hongqing Wang ◽  
...  
Keyword(s):  
High Performance Liquid Chromatography ◽  
Liquid Chromatography ◽  
Matrix Effect ◽  
Analytical Method ◽  
High Performance ◽  
Limit Of Detection ◽  
Solid Phase ◽  
Ammonium Hydroxide ◽  
Drug Residues ◽  
Protein Components

Abstract This study established a rapid and reliable method to determine chloramphenicol (CAP), thiamphenicol (TAP) and florfenicol (FF) residues in Chinese gelatin medicines. CAP, TAP and FF were extracted from medicine samples using 2% (v/v) ammonium hydroxide in acetonitrile. Trypsin was used to eliminate the matrix effect caused by protein components in gelatin medicines, whereas anhydrous sodium sulfate, C18-N and NH2-PSA adsorbents were applied to reduce matrix effect induced by other components. The analytical method of these drugs was optimized on ultra high-performance liquid chromatography-mass spectrometer (UHPLC-MS/MS) through the analysis of their standard linearity and regression. The optimized extraction and analytical method were validated in one Chinese gelatin medicine sample (Colla corii asini, E Jiao) with three fortification levels (2, 5 and 10 μg/kg), and the recoveries of these drug residues ranged of 87.6–102.7%. The limit of detection and quantification of CAP, TAP and FF in the sample were 0.2 and 0.5 μg/kg, 0.4 and 1.5 μg/kg, and 0.5 and 1.5 μg/kg, respectively. A total of 30 Chinese gelatin medicine samples were analyzed using the established method. No drug residues were found in these samples except for one Testudinis Carapacis et Plastri (1.67 μg/kg FF) and one turtle shell glue (2.55 μg/kg FF).

scholarly journals DEVELOPMENT OF A DIRECT METHOD OF ANALYZING TRANEXAMIC ACID LEVELS IN WHITENING CREAM USING REVERSED PHASE HIGH-PERFORMANCE LIQUID CHROMATOGRAPHY

2020 ◽  
pp. 88-92
Author(s):  
BAITHA PALANGGATAN MAGGADANI ◽  
JIHAN YASMINA ◽  
HARMITA HARMITA
Keyword(s):  
High Performance Liquid Chromatography ◽  
Liquid Chromatography ◽  
Tranexamic Acid ◽  
Analytical Method ◽  
High Performance ◽  
Limit Of Detection ◽  
Direct Method ◽  
Pharmaceutical Products ◽  
Optimal Method ◽  
Limit Of Quantitation

Objective: Whitening cream is a cosmetic that contains ingredients that can alleviate hyperpigmentation. Tranexamic acid (TA) is one of the potentialanti-pigmentation agents that work through inhibiting plasmin. TA is used in cosmetic formulations at a concentration of 2.5% as a whitening andmoisturizing agent. To date, research on TA in both cosmetics and other pharmaceutical products using high-performance liquid chromatography(HPLC) has not been done directly (without derivatization). Therefore, this study aimed to develop a simple and rapid analytical method for TA(without derivatization) in cosmetic cream samples using reverse-phase HPLC and water as a solvent.Methods: Optimization was conducted by evaluating several parameters that affect sample extraction, as well as composition and mobile phasetypes. The optimal method must fulfill suitability and validation requirements. The optimal method should be able to detect and quantify TA in creamsamples without derivatization.Results: The optimal analysis condition used a ultraviolet detector at a wavelength of 210 nm, acetonitrile: double-distilled water: phosphoric acid(64:34:2) as the mobile phase and a flow rate of 0.8 mL/min. The retention time of the analyte occurred in the 2nd min.Conclusion: The analytical method that met the validation requirements was characterized using parameters such as accuracy, precision, linearity,selectivity, limit, of detection, and limit of quantitation. This method is applicable for analyzing TA content in samples with a concentration of 1.02%.

scholarly journals HIGH-PERFORMANCE LIQUID CHROMATOGRAPHY ANALYTICAL METHOD VALIDATION FOR GLUTARALDEHYDE AND BENZALKONIUM CHLORIDE IN DISINFECTANTS

2018 ◽  
Vol 10 (1) ◽  
pp. 248
Author(s):  
Baitha Palanggatan Maggadani ◽  
Harmita . ◽  
Maizura Isfadhila
Keyword(s):  
High Performance Liquid Chromatography ◽  
Liquid Chromatography ◽  
Analytical Method ◽  
Benzalkonium Chloride ◽  
Mobile Phase ◽  
High Performance ◽  
Limit Of Detection ◽  
Analytical Method Validation ◽  
Limit Of Quantitation ◽  
Uv Visible

Objective: The aim of this study was to produce a selective, accurate, and faster high-performance liquid chromatography (HPLC) analytical methodfor benzalkonium chloride and glutaraldehyde in disinfectants using ultraviolet (UV)-visible detection.Methods: Glutaraldehyde has no chromophore, so it was first derivatized using 2,4 dinitro phenylhydrazine. Acetonitrile:water (75:25) was used asthe mobile phase for glutaraldehyde and acetonitrile-acetate pH 4 (75:25) for benzalkonium chloride, both at a flow rate of 1.2 mL/min. The optimizedassay was validated with respect to accuracy, precision, linearity, selectivity, limit of quantitation (LOQ), and limit of detection (LOD).Results: The method was linear for benzalkonium chloride, with correlation coefficient of 0.9995, LOD of 14.55 ppm, and LOQ of 48.51 ppm. Thecorrelation coefficient for glutaraldehyde was 0.9995, with LOD of 0.49 ppm and LOQ of 1.64 ppm. Accuracy was between 98% and 102%, andprecision was below 2% for both the tests.Conclusion: The HPLC analytical method for benzalkonium chloride and glutaraldehyde in disinfectants using UV-visible detection in this researchwas successful to produce a selective, accurate, and faster method.

scholarly journals Determination of Imazaquin Residues in Soil by Solid-Phase Extraction and High-Performance Liquid Chromatography

2007 ◽  
Vol 90 (2) ◽  
pp. 568-574 ◽  
Author(s):  
Chen Xuyan ◽  
Hu Jiye ◽  
Li Jianzhong
Keyword(s):  
High Performance Liquid Chromatography ◽  
Liquid Chromatography ◽  
Solid Phase Extraction ◽  
High Performance ◽  
Limit Of Detection ◽  
Solid Phase ◽  
Phase Extraction ◽  
Application Rates ◽  
Relative Standard ◽  
Strong Anion Exchange

Abstract A method has been developed for the quantitation of imazaquin residues in soil. The herbicide was extracted from soil with methanolwater (2 + 1, v/v) and cleaned up by strong anion-exchange solid-phase extraction cartridges. Analysis was performed by using high-performance liquid chromatography with ultraviolet detection. Average recoveries through the method ranged from 90.7 to 100.6%, with relative standard deviation equal to or lower than 6.6%. The limit of detection was estimated to be 0.0015 mg/kg, and the minimum quantitation concentration of imazaquin in soil was 0.005 mg/kg. This method was successfully applied to evaluate imazaquin residue levels in soil and its dissipation rates in a soybean field in the Xisanqi District of Beijing, People's Republic of China. The dissipation study showed that the half life of imazaquin in soil was 10.37 0.0135 days at 3 different application rates.

scholarly journals A NOVEL OF BEZAFIBRATE ANALYSIS METHODS IN URINE (IN VITRO) USING SOLID PHASE EXTRACTION– HIGH-PERFORMANCE LIQUID CHROMATOGRAPHY-UV DETECTOR

2018 ◽  
Vol 10 (1) ◽  
pp. 94
Author(s):  
Iyan Sopyan ◽  
Widiastuty Irawati ◽  
Wiwiek Indriyati
Keyword(s):  
High Performance Liquid Chromatography ◽  
Liquid Chromatography ◽  
Solid Phase Extraction ◽  
High Performance ◽  
Limit Of Detection ◽  
Solid Phase ◽  
Uv Detection ◽  
Phase Extraction ◽  
Uv Detector ◽  
Hydrophilic Lipophilic Balance

Objective: Bezafibrate is the second generation of fibrate groups used as the drug of choice in the treatment of hyperlipidemia. The purpose of this study is to obtained a validated method for analyzing bezafibrate in urine using solid phase extraction (SPE)-High performance liquid chromatography (HPLC).Methods: Solid phase extraction (SPE) using hydrophilic-lipophilic balance (HLB) cartridge was performed for bezafibrate extraction from urine, afterward, a validation of analysis method using high-performance liquid chromatography (HPLC)-(UV) detection was conducted to parameters, including: selectivity (Rs), linearity (r), accuracy, precision, limit of detection (LOD) and limit of quantification (LOQ). Results: Recovery extraction using SPE resulted %recovery 85-110%. The analysis was performed by high-performance liquid chromatography using reversed phase, C18 octadecylsilane (ODS) columns 250 x 26 mm, particle size 10 μl, with the composition of 0.01 M acetate buffer with pH 3.55: with percent composition (45:55) and 0.8 ml/minute on 230 nm UV detection. Validation includes selectivity, linearity, accuracy, precision LOD, and LOQ have fulfilled requirement value. Conclusion: The result of recovery extraction using SPE and validation of method exhibited the values that fulfilled the requirements and can be used for analysis bezafibrate in the urine.

scholarly journals METHOD DEVELOPMENT AND VALIDATION FOR ANALYSIS OF DEOXYARBUTININ ANHYDROUS EMULSION SYSTEM USING HIGH-PERFORMANCE LIQUID CHROMATOGRAPHY

2019 ◽  
pp. 172-175 ◽  
Author(s):  
MUCHTARIDI MUCHTARIDI ◽  
IDA MUSFIROH ◽  
AHMAD FAUZI
Keyword(s):  
High Performance Liquid Chromatography ◽  
Liquid Chromatography ◽  
Analytical Method ◽  
High Performance ◽  
Method Development ◽  
Limit Of Detection ◽  
Internal Standard ◽  
Emulsion System ◽  
Relative Standard ◽  
Limit Of Quantitation

Objective: The aim of this study is to develop a simple, precise and accurate analytical method of deoxyarbutin in anhydrous emulsion system preparation. Methods: The analysis was conducted using high-performance liquid chromatography (HPLC). Chromatographic analysis was carried out using a reversed phase-C18 column. The mobile consists of two phases methanol and water (60: 40 v/v) at a flow rate of 1.0 ml/min. The determinations were performed using UV detector set at 225 nm. All validation procedures were added with hydroquinone as an internal standard. Results: The method showed coefficient correlation is 0.9978, relative standard deviation (RSD) smaller than 2%, Limit of Detection (LOD) and Limit of Quantitation (LOQ) are 0.599 µg/ml and 1.817 µg/ml respectively. The total amount deoxyarbutin in anhydrous emulsion preparation is 1.964+0.02 % with 98% recovery percentage. Conclusion: The developed HPLC analytical method meets the validation criteria made by International Conference on Harmonisation (ICH).

Packed-nanofiber solid phase extraction coupled with HPLC for the determination of chloramphenicol in milk

2017 ◽  
Vol 9 (46) ◽  
pp. 6499-6506 ◽  
Author(s):  
Lanling Chu ◽  
Jianjun Deng ◽  
Xuejun Kang
Keyword(s):  
High Performance Liquid Chromatography ◽  
Liquid Chromatography ◽  
Solid Phase Extraction ◽  
Analytical Method ◽  
High Performance ◽  
Solid Phase ◽  
Phase Extraction

A sensitive analytical method based on packed-nanofiber solid phase extraction (PFSPE) and high performance liquid chromatography (HPLC) has been developed for determining chloramphenicol (CAP) in milk.

scholarly journals Phytochemical Analysis of Twelve Marker Analytes in Sogunjung-tang Using a High-Performance Liquid Chromatography Method

2020 ◽  
Vol 10 (23) ◽  
pp. 8561
Author(s):  
Chang-Seob Seo ◽  
Hyeun-Kyoo Shin
Keyword(s):  
High Performance Liquid Chromatography ◽  
Liquid Chromatography ◽  
Formic Acid ◽  
Analytical Method ◽  
High Performance ◽  
Limit Of Detection ◽  
Array Detector ◽  
Phytochemical Analysis ◽  
Limit Of Quantification ◽  
Chromatography Method

Sogunjung-tang (SGJT) is a traditional herbal prescription that has been used in Korea for the treatment of abdominal pain since ancient times. In this study, an analytical method for the simultaneous quantification of 12 marker analytes (gallic acid (GA), albiflorin (ALB), paeoniflorin (PAE), liquiritin apioside (LIAP), liquiritin (PIQ), benzoic acid (BA), coumarin (COU), liquiritigenin (LIQG), cinnamic acid (CINA), benzoylpaeoniflorin (BPAE), cinnamaldehyde (CINAD), and glycyrrhizinic acid (GLYA)) for quality evaluation of SGJT was developed based on high-performance liquid chromatography (HPLC) combined with a photodiode array detector. A Waters SunFire reverse-phased C18 column was used for the chromatographic separation of the 12 marker analytes in SGJT using a two-mobile phases system consisting of 0.1% (v/v) aqueous formic acid and 0.1% (v/v) formic acid in acetonitrile. The developed analytical method was validated by assessment of linearity, limit of detection, limit of quantification, recovery, and precision. Using the developed and validated HPLC method, the 12 marker analytes were determined to be present in 0.10–32.83 mg/g in SGJT.

scholarly journals SEPARATION AND DETERMINATION OF THE R-ISOMER OF ETODOLAC IN A BULK DRUG SUBSTANCE BY NORMAL-PHASE LIQUID CHROMATOGRAPHY

2016 ◽  
Vol 9 (6) ◽  
pp. 327
Author(s):  
Appasaheb Bajirao Lawande
Keyword(s):  
High Performance Liquid Chromatography ◽  
Liquid Chromatography ◽  
Analytical Method ◽  
Mobile Phase ◽  
High Performance ◽  
Limit Of Detection ◽  
Normal Phase ◽  
Limit Of Quantification ◽  
Bulk Drug

ABSTRACT Objective:  The objective of the this work is to develop and validate a novel, simple,rapid and reliable analytical method for separation and determination of R-isomer impurity in Etodolac bulk drug material by normal-phase high-performance liquid chromatography as per International Conference on Harmonization guidelines. Methods: The Etodolac R- isomer and S-isomer were separated on a Chiralcel OD-H (150 x 4.0 mm, 5 micron) column by using Ethanol : n-Hexane:Trifluoroacetic acid (50:50:0.1 v/v.) mobile phase with equipped detector at wavelength 225 nm and 25 °C column oven temperature. The resolution between R-isomer and S-isomer were more than two recorded on chromatogram. The specified method was developed and validated for various parameters like reproducibility, limit of detection, limit of quantification, linearity and range, robustness, solution stability and mobile phase stability according to the International Conference on Harmonization (ICH) guidelines.  Results: Linearity were found for Etodolac R-isomer over the concentration range of 600–6000 ng/ml, with the linear regression (Correlation coefficient R = 0.998) and proved to be robust. Limit of detection and limit of quantification of Etodolac R-isomer was found to be 200 and 600 ng/ml. The retention time of R-isomer was considered to be 2.8 min. The percentage recovery of Etodolac R-isomer has been ranged from 97.0 to 102.0 in bulk drug material sample. The proposed analytical method has been found to be suitable, precise,reliable and accurate for the separation and quantitative determination of Etodolac R-isomer in bulk drug sample.                                                                                                                   Conclusion: A novel, speedy, accurate, precise, reliable and rugged analytical method has been developed and validated for normal phase high performance liquid chromatography to determine R-isomer impurity in Etodolac bulk drugs material as per ICH guideline. Keywords: Etodolac, HPLC, Known Impurity. Normal Phase, Validation.

scholarly journals ANALYSIS OF FERULIC ACID IN ARABICA COFFEE BEAN (COFFEA ARABICA L.) USING SOLID PHASE EXTRACTION–HIGH PERFORMANCE LIQUID CHROMATOGRAPHY

2019 ◽  
pp. 151-155
Author(s):  
IDA MUSFIROH ◽  
WIWIEK INDRIYATI ◽  
MIRA LAILA NUR ABADI ◽  
MUCHTARIDI MUCHTARIDI
Keyword(s):  
High Performance Liquid Chromatography ◽  
Liquid Chromatography ◽  
Solid Phase Extraction ◽  
Ferulic Acid ◽  
High Performance ◽  
Limit Of Detection ◽  
Solid Phase ◽  
Phase Extraction ◽  
Coffee Bean ◽  
Arabica Coffee

Objective: The purpose of this research is quantitatively analyzing of ferulic acid in the Arabica coffee bean extract from three samples with different regions (Garut, Pangalengan, Tasikmalaya, West Java Indonesia) using Solid Phase Extraction-High Performance Liquid Chromatography (SPE-HPLC) method which is validated. Methods: The analysis method used reversed phase HPLC with an Enduro C 18 G (250 mm × 4.6 mm) column and detector UV 312 nm, with a mobile phase of methanol and water containing 1% (v/v) of acetic acid (42:58) at a flow rate of 1.0 ml/min and validation method was examined in linearity, Limit of Detection (LOD), Limit of Quantification (LOQ), precision, and accuracy. Results: The results showed that the precision of retention was 8.853 min, correlation coefficient (R) was 0.9996, and the recovery was 96.909%. The quantitative analysis of ferulic acid content in the extract of coffee from thus samples of three different regions were 0.0385%, 0.0169% and 0.0076%, respectively. Conclusion: The analytical method was meet the validation criteria. Ferulic acid levels results from the extraction of the digestion process and pretreatment methods of Solid Phase Extraction (SPE) is 0.0385% from Garut area, 0.0169% from Pangalengan area and 0.0076% from Tasikmalaya area.

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