scholarly journals Withdrawal Interval Estimation of Doxycycline in Yellow Catfish (Pelteobagrus fulvidraco) Using an LC-MS/MS Method Based upon QuEChERS Sampling Preparation

Foods ◽  
2021 ◽  
Vol 10 (11) ◽  
pp. 2554
Author(s):  
Ning Xu ◽  
Bo Cheng ◽  
Miao Li ◽  
Zhoumeng Lin ◽  
Xiaohui Ai
Keyword(s):  
Limit Of Detection ◽  
Interval Estimation ◽  
Pelteobagrus Fulvidraco ◽  
Aquatic Animal ◽  
Limited Information ◽  
Yellow Catfish ◽  
Simple Method ◽  
Tissue Samples ◽  
Limit Of Quantitation

Limited information on residue depletion of doxycycline (DC) is available in yellow catfish (Pelteobagrus fulvidraco) using the determination of LC-MS/MS based upon a rapid and simple method of sample preparation. This study collected plasma and tissue samples of yellow catfish at pre-determined time points following 3-day consecutive oral administration of DC at 20 mg/kg. The samples were prepared using a QuEChERS (Quick, Easy, Cheap, Effective, Rugged, and Safe) approach. The limit of detection and the limit of quantitation were 2.5 and 5 µg/kg or µg/L, respectively, for DC in plasma and tissues (e.g., muscle + skin, liver, kidney, and gill). The recoveries of DC ranged from 67.2% to 86.2%. The decision limit (CCα) and the detection capability (CCβ) were from 106.2 to 127.8 μg/kg or μg/L. The withdrawal times of DC in muscle + skin were estimated to be 22 d based on the guidelines in China and Europe and 27 d based on Japan’s standard. Overall, this study not only provides an efficient method to rapidly determine the DC concentrations in fish-derived tissues but also provides important information on the safety assessment of DC in aquatic animal-derived food products.

Rapid and Simple Method for Isolation and Gas Chromatographic Determination of N-Nitrosodimethylamine in Dimethyldithiocarbamate Formulations

1989 ◽  
Vol 72 (4) ◽  
pp. 663-666
Author(s):  
Yuk Y Wigfield ◽  
Charles C Mclenaghan
Keyword(s):  
Thermal Energy ◽  
Limit Of Detection ◽  
Chromatographic Determination ◽  
Energy Analyzer ◽  
Organic Fraction ◽  
Gas Chromatograph ◽  
Simple Method ◽  
Limit Of Quantitation ◽  
Extraction Tube

Abstract A rapid and simple method to isolate and determine JV-nitrosodimethylamine (NDMA) in formulations of ferbam or dibam has been developed. Depending on the type of formulation, the sample is extracted or diluted with water which is subsequently extracted with dichloromethane. NDMA is isolated by passing the organic fraction through a silica gel column and eluting the column with acetone. The acetone eluate is analyzed directly for NDMA by using a gas chromatograph connected to a thermal energy analyzer detector (GC/ TEA). The limit of detection (LOD) is 40 pg (0.04 ppm) and the limit of quantitation (LOQ) is 100 pg (0.1 ppm). The recovery range for this method is 85-112% for ferbam spiked at 0.33-0.75 ppm, and 91- 113% for dibam spiked at 0.32-1.09 ppm. Sixteen commercial samples of ferbam and 4 of dibam were analyzed; one ferbam sample contained 19.8 ppm NDMA while all others contained less than 1 ppm. Chem-Elut extraction tubes were found to generate trace quantities of nitrosamine from samples containing amine. If amine is absent, an extraction tube could be used in place of dichloromethane extraction to give similar values in recovery range, LOD, and LOQ.

Simultaneous Determination of Four Herbicide and Pesticide Residues in Chinese Green Tea Using QuEChERS Purification Procedure and UPLC-MS/MS Analysis

2013 ◽  
Vol 634-638 ◽  
pp. 1586-1590
Author(s):  
Su Fang Wang ◽  
Shou Jie Zhang ◽  
Chun Hong Dong ◽  
Guo Qing Wang ◽  
Jun Feng Guo ◽  
...  
Keyword(s):  
Formic Acid ◽  
Simultaneous Determination ◽  
Green Tea ◽  
Limit Of Detection ◽  
Multiple Reaction Monitoring ◽  
Graphitized Carbon Black ◽  
Ms Analysis ◽  
Relative Standard ◽  
Limit Of Quantitation

A method for simultaneous determination of residuals of four herbicides and pesticides, simazine, carboxin, diflubenzuron and rotenone, in Chinese green tea was developed. In the proposed method, the tea powder was placed in a centrifuge tube with a plug, extracted in saturated aqueous sodium chloride solution and acetonitrile, agitated using vortex oscillator, and then centrifuged 5 min at 4000 rpm. The supernatant solution was purified by primary secondary amine (PSA) sorbent, C18 power, and graphitized carbon black powder, respectively. Then the purified extracts were dissolved with acetonitrile:0.1% formic acid aqueous solution (40:60, V/V) and agitated, filtered using a syringe with 0.22 μm nylon filter prior to UPLC-MS/MS analysis. The UPLC analysis was performed on an ACQUITY UPLC® HSS T3 column (2.1 mm×100 mm, 1.8 µm), using acetonitrile-0.1% formic acid as mobile phase with the flow rate as 0.3 mL•min-1. Injection volume was 10 µL. Positive ionization mode was applied, and the ions were monitored in the multiple reaction monitoring (MRM) mode with curtain gas 0.069 MPa, collision gas 0.052 MPa, ESI ion spray voltage 5000 V, temperature 550 °C, nebulizer gas 0.24 MPa, and turbo gas 0.28 MPa. The limit of detection (LOD) and limit of quantitation (LOQ) of the proposed method are 1 μg•kg-1and 5 μg•kg-1, respectively. The average recoveries of the four pesticides at 10, 20, and 50 µg•kg-1spiking levels range from 77.4% to 95.3%. TheSupersSuperscript textcript textrelative standard deviation (RSD) (n=6) range form 11.83% to 4.52%.

scholarly journals STABILITY INDICATING HPLC METHOD FOR DETERMINATION OF VILAZODONE HYDROCHLORIDE

2017 ◽  
Vol 9 (4) ◽  
pp. 123
Author(s):  
Birva A. Athavia ◽  
Zarna R. Dedania ◽  
Ronak R. Dedania ◽  
S. M. Vijayendra Swamy ◽  
Chetana B. Prajapati
Keyword(s):  
Limit Of Detection ◽  
Degradation Products ◽  
Hplc Method ◽  
Alkaline Condition ◽  
Forced Degradation ◽  
Molecular Formula ◽  
Stability Indicating ◽  
Dry Heat ◽  
Limit Of Quantitation

Objective: The aim and objective of this study was to develop and validate Stability Indicating HPLC method for determination of Vilazodone Hydrochloride.Methods: The method was carried out on a Phenomenex, C18 (250x4.6 mm, 5 µm) Column using a mixture of Acetonitrile: Water (50:50v/v), pH adjusted to 3.3 with Glacial Acetic Acid for separation. The flow rate was adjusted at 1 ml/min and Detection was carried out at 240 nm.Results: The retention time of vilazodone hydrochloride was found to be 2.3 min. The calibration curve was found to be linear in the range 25-75µg/ml with a correlation coefficient (R2=0.996). The limit of detection and limit of quantitation were found to be 4.78µg/ml and 14.48µg/ml respectively. The % recovery of vilazodone hydrochloride was found to be in the range of 98.21±0.08 % to 99.07±0.64%. The proposed method was successfully applied for the estimation of vilazodone hydrochloride in marketed tablet formulation.Vilazodone Hydrochloride was subjected to forced degradation under Acidic, Alkaline, Oxidation, Dry Heat and Photolytic degradation conditions. Vilazodone hydrochloride showed 3.12% degradation under acidic condition, 4.78% under alkaline condition, 7.8% under oxidation condition, 3.53% under dry heat condition and 4.9% under photolytic condition.Acid degradation impurity was identified and characterised by LC-MS/MS was found to be 1-(4-Penten-1-yl) piperazine having molecular weight 154.253 (m/z 155.08) and Molecular Formula C9H18N2.Conclusion: A simple, precise, rapid and accurate Stability Indicating HPLC method has been developed and validated for the determination of Vilazodone Hydrochloride in presence of its degradation products as per the ICH Guidelines. 

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 Determination of Simvastatin by Voltammetry Method at Screen-Printed Electrode Modified by Graphene Oxide Nanosheets and Sodium Dodecyl Sulfate

2022 ◽  
Author(s):  
Abolfazl Darroudi ◽  
Saeid Nazari ◽  
Seyed Ali Marashi ◽  
Mahdi Karimi-Nazarabad
Keyword(s):  
Graphene Oxide ◽  
Sodium Dodecyl Sulfate ◽  
Limit Of Detection ◽  
Sodium Dodecyl ◽  
Screen Printed Electrode ◽  
Support Electrolyte ◽  
Limit Of Quantitation ◽  
Dodecyl Sulfate ◽  
Screen Printed

Abstract An accurate, rapid, simple, and novel technique was developed to determine simvastatin (SMV). In this research, a screen-printed electrode (SPE) was deposited with graphene oxide (GO) and sodium dodecyl sulfate (SDS), respectively. For the first time, the handmade modified SPE measured the SMV by differential pulse voltammetry (DPV) with high sensitivity and selectivity. The results of cyclic voltammetry indicated the oxidation irreversible process of SMV. Various parameters (pH, concentration, scan rate, support electrolyte) were performed to optimize the conditions for the determination of SMV. Under the optimum experiment condition of 0.1 M KNO3 as support electrolyte and pH 7.0, the linear range was achieved for SMV concentration from 1.8 to 36.6 µM with a limit of detection (LOD), and a limit of quantitation (LOQ) of 0.06 and 1.8 µM, respectively. The proposed method was successfully utilized to determine SMV in tablets and urine samples with a satisfactory recovery in the range of 96.2 to 103.3%.

scholarly journals Spectrophotometric Determination of Olmutinib in Bulk by Area under Curve and First Order Derivative Methods and its Validation as per ICH guidelines

2019 ◽  
Vol 9 (4-A) ◽  
pp. 349-354
Author(s):  
BALU KHANDARE ◽  
Atish C. Musle ◽  
Sanket S. Arole ◽  
Pravin V. Popalghat
Keyword(s):  
Area Under Curve ◽  
Limit Of Detection ◽  
Order Derivative ◽  
Spectrometric Method ◽  
First Order ◽  
Accuracy And Precision ◽  
Ich Guidelines ◽  
Validation Parameters ◽  
Limit Of Quantitation

Abstract: A simple, precise and economical UV-spectrophotometric method has been developed for the estimation of Olmutinib from bulk. Two methods were developed First method (A) applied was area under curve (AUC) in which the area was integrated in wavelength from 262-272nm. Second method (B) was first order derivative spectrometric method. In this method absorbance at λmin=256.57nm, λmax=282.83nm and zero cross=267.68nm was measured. Calibration curves were plotted for the method by using instrumental response at selected wavelength and concentration of analyte in the solution. In both the methods, linearity was observed in the concentration range of 2-12µg/ml at the λmax=267.68nm. Accuracy and precision studies were carried out and results were satisfactorily obtained. The drug at each of the 80 %, 100 % and 120 % levels showed good recoveries that is in the range of 98.00 to 99.00% for both methods, hence it could be said that the method was accurate. Limit of detection (LOD) and limit of quantitation (LOQ) were determined for the method. The method was validated as per International Conference on Harmonization. All validation parameters were within the acceptable limit. The developed method was successfully applied to estimate the amount of Olmutinib in pharmaceutical formulation.

scholarly journals Liquid Chromatographic Determination of α-Solasonine in Frozen Green Peas as an Indicator of the Presence of Nightshade Berries

2003 ◽  
Vol 86 (4) ◽  
pp. 759-763 ◽  
Author(s):  
Peter Cavlovic ◽  
Mohan Mankotia ◽  
Peter Pantazopoulos ◽  
Peter M Scott
Keyword(s):  
Limit Of Detection ◽  
Chromatographic Determination ◽  
Solanum Nigrum ◽  
Expanded Uncertainty ◽  
Method Performance ◽  
Limit Of Quantitation ◽  
Liquid Chromatographic Determination ◽  
Liquid Chromatographic ◽  
Green Peas

Abstract Nightshade berries containing glycoalkaloids can be a contaminant in green peas. Methodology was developed to detect this contamination. The glycoalkaloid α-solasonine was extracted from frozen green peas with 1% (v/v) acetic acid, cleaned up on a C18 cartridge, and determined by liquid chromatography with UV detection at 200 nm. Method performance characteristics for the determination of α-solasonine include linearity from 140 to 1500 ng injected (r = 0.9996–0.9999); recovery ranging from 68 to 79%; limit of quantitation (LOQ) = 4.5 ppm (280 ng standard), and limit of detection = 0.64 ppm (40 ng standard). At the LOQ, the expanded uncertainty at 95% confidence was 0.38 × the reported value. The method was applied to the detection of α-solasonine in frozen green peas in a 2-year study of 60 samples of frozen green peas from Ontario, Canada. None of the samples contained α-solasonine. No unripe berries of Solanum nigrum were detected visually in the samples.

scholarly journals Determination of Vitamin K1 in Medical Foods by Liquid Chromatography with Postcolumn Reduction and Fluorometric Detection

2000 ◽  
Vol 83 (4) ◽  
pp. 957-962 ◽  
Author(s):  
George M Ware ◽  
G William Chase ◽  
Ronald R Eitenmiller ◽  
Austin R Long
Keyword(s):  
Limit Of Detection ◽  
Solid Phase ◽  
Sodium Bicarbonate Solution ◽  
Reversed Phase ◽  
Mean Value ◽  
Fluorometric Detection ◽  
Vitamin K1 ◽  
Limit Of Quantitation ◽  
Medical Foods

Abstract A liquid chromatographic (LC) method is described for the determination of vitamin K1 in medical foods. The sample is enzymatically digested with lipase and α-amylase and extracted with 1% sodium bicarbonate solution–isopropanol (1 + 1). After C18 solid-phase extraction, vitamin K1 is separated by nonaqueous reversed-phase LC, converted to the hydroquinone by postcolumn zinc reduction, and quantitated by fluorescence detection. The limit of detection is 8 pg (3 σ), and the limit of quantitation is 27 pg (10 σ) on column. Linear response ranged from 0.1 to 1.0 ng vitamin K1 (r = 0.9999). The mean recovery (n = 38) for all spiking levels was 101.6 ± 2.85%. Analysis of Standard Reference Material 1846, Infant Formula, gave a mean value of 0.95 ± 0.088 mg vitamin K/kg (K or K1?)(n = 31) with a coefficient of variation of 9.26.

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 Determination of 7B3 Residues in Cotton Plants by Liquid Chromatography/Mass Spectrometry

2009 ◽  
Vol 92 (1) ◽  
pp. 302-306 ◽  
Author(s):  
Xiao-Jing Yan ◽  
Xiao-Mei Liang ◽  
Yan-Jun Xu ◽  
Shu-Hui Jin ◽  
Dao-Quan Wang
Keyword(s):  
Mass Spectrometry ◽  
Liquid Chromatography ◽  
Limit Of Detection ◽  
Reversed Phase ◽  
Liquid Chromatography Mass Spectrometry ◽  
Chromatography Mass Spectrometry ◽  
Relative Standard ◽  
Limit Of Quantitation ◽  
Cotton Plants

Abstract A method was developed for the determination of 7B3 (12-propyloxyimino-1,15-pentadecanlactam), a novel macrolactam fungicide, by liquid chromatography/mass spectrometry (LC/MS) with positive electrospray ionization (ESI+). The method used a reversed-phase C18 column and acetonitrilewater (60 + 40, v/v) mobile phase. The quick, easy, cheap, effective, rugged, and safe method was used for extraction of 7B3 from cotton plants, which involved the extraction of 10 g homogenized sample with 10 mL acetonitrile, followed by the addition of 4 g anhydrous MgSO4 and 1.0 g NaCl. After centrifugation, 1 mL of the buffered acetonitrile extract was transferred into a tube containing 50 mg primary secondary amine sorbent and 100 mg anhydrous MgSO4. After shaking and centrifugation, the final extract was transferred to an autosampler vial for concurrent analysis by LC/MS. The results of 7B3 determined by LC/MS in the selective ion monitoring mode were linear, and the matrix effect of the method was evaluated. The average recoveries of 7B3 fortified at different levels were within 84.1100.2, and the relative standard deviations were <7.5 for all samples analyzed. The method limit of detection and the limit of quantitation values were 0.03 and 0.1 mg/kg, respectively. The proposed method was successfully applied to determine 7B3 residues in practical samples. This method is sensitive, accurate, reliable, simple, and safe.

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