scholarly journals Determination of Pantothenic Acid in Foods by Optical Biosensor Immunoassay

2005 ◽  
Vol 88 (4) ◽  
pp. 1008-1014 ◽  
Author(s):  
Simon A Haughey ◽  
Anthony A O'Kane ◽  
G Andrew Baxter ◽  
Andras Kalman ◽  
Marie-José Trisconi ◽  
...  
Keyword(s):  
Limit Of Detection ◽  
Extraction Procedure ◽  
Pantothenic Acid ◽  
Optical Biosensor ◽  
Liquid Chromatography Mass Spectrometry ◽  
Relative Standard ◽  
Wide Range ◽  
Simple Extraction ◽  
Reference Samples

Abstract An optical biosensor inhibition immunoassay was developed using a specific pantothenic acid-binding protein for the quantitation of free pantothenic acid (vitamin B5) in foodstuffs. Samples were prepared by a simple extraction procedure in buffer, and vitamin content was estimated against authentic calibrants in the same buffer. Performance parameters included a working range of 10–5000 ng/mL, a limit of detection of 4.4 ng/mL, precision relative standard deviation of 5.4–7.1% over a range of concentrations, and recoveries >95% in the matrixes tested. A wide range of foodstuffs, including National Institute of Standards and Technology reference samples, were tested in 3 independent laboratories and the results were compared with microbiological assay and liquid chromatography/mass spectrometry (LC/MS) methods. The results indicate that the biosensor technique is appropriate for the estimation of pantothenic acid in a wide range of foodstuffs.

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.

Radioisotope Dilution Technique for Determination of Vitamin B12 in Foods

1982 ◽  
Vol 65 (1) ◽  
pp. 85-88 ◽  
Author(s):  
Patrick J Casey ◽  
Keevin R Speckman ◽  
Frank J Ebert ◽  
William E Hobbs
Keyword(s):  
Standard Deviation ◽  
Vitamin B12 ◽  
Relative Standard Deviation ◽  
Extraction Procedure ◽  
Dilution Technique ◽  
Microbiological Method ◽  
Relative Standard ◽  
Wide Range ◽  
The Mean

Abstract A radioisotope dilution (RID) method for the determination of vitamin B12 is presented. The method combines a standard extraction procedure (AOAC 43.108,12th ed.) with a commercially available RID assay kit. The method was evaluated on a wide range of fortified and unfortified food products. Recovery studies on both groups yielded average recoveries of 98.1 and 95.8%, respectively. Reproducibility data generated from replicate analyses on both groups gave a relative standard deviation of 6.9% for the fortified group and 9.2% for the unfortified group. For the samples studied, the mean vitamin B12 content determined by the RID method was 8.01 μg/100 g vs imean of 7.54 μg/100 g by the AOAC microbiological method; the correlation coefficient was r = 0.983.

scholarly journals Spectrophotometric Determination of Iron(II) after Solid Phase Extraction of Its 2,2′ Bipyridine Complex on Silica Gel-Polyethylene Glycol

2013 ◽  
Vol 2013 ◽  
pp. 1-6 ◽  
Author(s):  
Nahid Pourreza ◽  
Saadat Rastegarzadeh ◽  
Ali Reza Kiasat ◽  
Hossein Yahyavi
Keyword(s):  
Polyethylene Glycol ◽  
Solid Phase Extraction ◽  
Silica Gel ◽  
Limit Of Detection ◽  
Solid Phase ◽  
Extraction Procedure ◽  
Calibration Graph ◽  
Phase Extraction ◽  
Relative Standard

A new solid phase extraction procedure was developed for preconcentration of iron(II) using silica gel-polyethylene glycol (silica-PEG) as an adsorbent. The method is based on retention of iron(II) as 2,2′ bipyridine complex on silica-PEG. The retained complex is eluted by 1.0 mol L−1of sulfuric acid-acetone mixture (1:2) and its absorbance is measured at 518 nm, spectrophotometrically. The effects of different parameters such as pH, concentration of the reagent, eluting reagent, sample volume, amount of adsorbent, and interfering ions were investigated. The calibration graph was linear in the range of 1–60 ng mL−1of iron(II). The limit of detection based on3Sbwas 0.57 ng mL−1and relative standard deviations (R.S.D) for ten replicate measurements of 12 and 42 ng mL−1of iron(II) were 2.4 and 1.7%, respectively. The method was applied to the determination of of iron(II) in water, multivitamin tablet, and spinach samples.

Determination of Oxyfluorfen Herbicide and Oxyfluorfen Amine Residues in Garbanzo Beans by Liquid Chromatography

1991 ◽  
Vol 74 (3) ◽  
pp. 546-550
Author(s):  
Min Zhou ◽  
Carl J Miles
Keyword(s):  
Gas Chromatography ◽  
Liquid Chromatography ◽  
Ion Chromatography ◽  
Standard Method ◽  
Extraction Procedure ◽  
Detection Limits ◽  
Analysis Time ◽  
Wide Range ◽  
Simple Extraction

Abstract Oxyfluorfen and oxyfluorfen amine were determined by liquid chromatography (LC) with ultraviolet (UV) and photoconductivity detection (PCD). A simple extraction procedure acceptably recovered both analytes from garbanzo beans over a wide range of fortifications (0.05 to 20 ppm) (83 ± 4 for oxyfluorfen; 85 ± 4 for oxyfluorfen amine). Percent recoveries decreased slightly as the fortification level decreased. Both analytes could be determined simultaneously at a concentration >0.2 ppm In garbanzo beans. Detection limits were 3 ng for oxyfluorfen and 100 ng for oxyfluorfen amine using LC/UV, and 12 ng for both oxyfluorfen and oxyfluorfen amine with LC/PCD. Different knitted reaction coils and photoreactors were evaluated. Photoproduct yields and Identification were determined by ion chromatography. The LC/PCD method measures oxyfluorfen and oxyfluorfen amine separately and has a shorter analysis time, while the standard method using gas chromatography measures total residues and is more sensitive.

Determination of Histamine in Fish by Liquid Chromatography with Post-Column Reaction and Fluorometric Detection

1984 ◽  
Vol 67 (6) ◽  
pp. 1040-1043
Author(s):  
Milda J Walters
Keyword(s):  
Limit Of Detection ◽  
Detection Sensitivity ◽  
Fluorometric Detection ◽  
Canned Tuna ◽  
Relative Standard ◽  
Cation Exchange Column ◽  
Aoac Method ◽  
Simple Extraction ◽  
Liquid Chromatographic

Abstract A liquid chromatographic (LC) system, using a bonded cation-exchange column, resolves histamine from histidine and other related compounds. Detection sensitivity and specificity are enhanced by introduction of a post-column reaction with o-phthalaldehyde to form a fluorescent derivative. The limit of detection is 1.5 ng histamine, and the response is linear over a range of 7-750 ng. The average histamine recovery from fortified tuna and mahimahi samples was 98.4% with a relative standard deviation of 2.18%. The results for canned tuna and mahimahi were comparable to those obtained by using the official AOAC method. The LC method requires only simple extraction of the sample before introduction into the LC system, which resolves and detects cadaverine and putrescine in addition to histamine.

scholarly journals Extraction and Determination of Amygdaline in Iraqi Plant Seeds Using the Combined Simple Extraction Procedure and High-Performance Liquid Chromatography

2013 ◽  
Vol 10 (2) ◽  
pp. 350-361
Author(s):  
Baghdad Science Journal
Keyword(s):  
High Performance Liquid Chromatography ◽  
Liquid Chromatography ◽  
High Performance ◽  
Limit Of Detection ◽  
Extraction Procedure ◽  
Reversed Phase ◽  
Plant Seeds ◽  
Relative Standard ◽  
Limit Of Quantitation ◽  
Simple Extraction

Abstract :In this study, amygdaline in Iraqi plant seeds was extracted and isolated from their seeds matrix using reflux procedure and subsequently identified and determined by high performance liquid chromatography (HPLC) on reversed phase column of LC-18 (150mm x 4.6mm, 5?m )with actonitrile :water ( 50 : 50 ) as mobile phase at flow rate of ( 0.5 mL/min ) and detection at wavelength of 215 nm.The experimental results indicated that the linearity of calibration is in the range of 1.0-30.0 mg L-1amygdaline with the correlation coefficient of 0.9949. The limit of detection (LOD) and limit of quantitation (LOQ) for amygdaline were of 0.88 and 2.93 mg L-1 in standard pure sample. The mean recovery percent is 97.34±0.58 at 95% confidence interval and relative standard deviation in the range of 1.19-2.08 %. The content of amygdaline in plant samples was 4.60± 0.47 g /100 g, and 0.27±0.029 g/100g of apricot and citrullus colocynth respectively.

scholarly journals MICELLAR ENHANCED SYNCHRONOUS FLUORESCENCE FOR THE ASSAY OF SUMATRIPTAN SUCCINATE IN PHARMACEUTICAL TABLETS

2019 ◽  
pp. 218-223
Author(s):  
SAFWAN M. FRAIHAT
Keyword(s):  
Limit Of Detection ◽  
Fluorescence Emission ◽  
Reference Method ◽  
Synchronous Fluorescence ◽  
Pharmaceutical Tablets ◽  
Sumatriptan Succinate ◽  
Accuracy And Precision ◽  
Relative Standard ◽  
Wide Range

Objective: To develop a sensitive, fast and selective method for the determination of sumatriptan succinate (SUM) in pharmaceutical samples. Methods: The method is based on measuring the synchronous fluorescence of SUM using ∆λ of (120 nm) and at a wavelength of excitation and emission of 230 and 325 nm respectively, using Agilent Technology, Cary eclipse, G9800AA model Luminescence spectrometer. Effect of variables on fluorescence emission intensities was studied such as solvent, surfactant, and pH. The proposed method was validated in term of linearity, limit of detection as per the international conference on harmonization guidelines ICH Q2 (R1). Results: The linearity of the method was obtained with a wide range of (50-150) ng/ml with a high value of correlation coefficient value of (0.992). Limits of detection (LOD) and limits of quantitation (LOQ) were found to be 16.3 and 49.5 ng/ml respectively, the mean recovery was found to be 99.1% with low relative standard deviation (% RSD). The method was also compared statistically with the reference method using t-test and f-test, the results show no difference either in pure or pharmaceutical tablets. Conclusion: The obtained results revealed that the developed method can be applied successfully for the determination of SUM in drug formulations samples with good accuracy and precision.

scholarly journals A novel LC-MS method development and validation for the determination of phenyl vinyl sulfone in eletriptan hydrobromide

2021 ◽  
Vol 7 (1) ◽  
Author(s):  
Indhu Priya Mabbu ◽  
G. Sumathi ◽  
N. Devanna
Keyword(s):  
Method Development ◽  
Limit Of Detection ◽  
Vinyl Sulfone ◽  
Limit Of Quantification ◽  
Relative Standard ◽  
Pressure Chemical Ionization ◽  
Pressure Chemical ◽  
Development And Validation ◽  
Phenyl Vinyl

Abstract Background The aim of the present method is to develop and validate a specific, sensitive, precise, and accurate liquid chromatography-mass spectrometry (LC-MS) method for the estimation of the phenyl vinyl sulfone in the eletriptan hydrobromide. The effective separation of the phenyl vinyl sulfone was achieved by the Symmetry C18 (50 × 4.6 mm, 3.5 μm) column and a mobile phase composition of 0.1%v/v ammonia buffer to methanol (5:95 v/v), using 0.45 ml/min flow rate and 20 μl of injection volume, with methanol used as diluent. The phenyl vinyl sulfone was monitored on atomic pressure chemical ionization mode mass spectrometer with positive polarity mode. Results The retention time of phenyl vinyl sulfone was found at 2.13 min. The limit of detection (LOD) and limit of quantification (LOQ) were observed at 1.43 ppm and 4.77 ppm concentration respectively; the linear range was found in the concentration ranges from 4.77 to 27.00 ppm with regression coefficient of 0.9990 and accuracy in the range of 97.50–102.10%. The percentage relative standard deviation (% RSD) for six replicates said to be injections were less than 10%. Conclusion The proposed method was validated successfully as per ICH guidelines. Hence, this is employed for the determination of phenyl vinyl sulfone in the eletriptan hydrobromide.

scholarly journals Rapid Determination of Ethylene Oxide and 75 VOCs in Ambient Air with Canister Sampling and Associated Growth Issues

Separations ◽  
2021 ◽  
Vol 8 (3) ◽  
pp. 35
Author(s):  
Jason Hoisington ◽  
Jason S. Herrington
Keyword(s):  
Ethylene Oxide ◽  
Rapid Determination ◽  
Complex Mixture ◽  
Ambient Air ◽  
Gas Chromatography Mass Spectrometry ◽  
Average Accuracy ◽  
Relative Standard ◽  
Wide Range ◽  
Us Epa

A canister-based sampling method along with preconcentrator-Gas chromatography-Mass Spectrometry (GC-MS) analysis was applied to ethylene oxide (EtO or EO) and 75 other volatile organic compounds (VOCs) in ambient air. Ambient air can contain a large variety of VOCs, and thorough analysis requires non-discriminatory sampling and a chromatographic method capable of resolving a complex mixture. Canister collection of whole air samples allows for the collection of a wide range of volatile compounds, while the simultaneous analysis of ethylene oxide and other VOCs allows for faster throughput than separate methods. The method presented is based on US EPA Method TO-15A and allows for the detection of EtO from 18 to 2500 pptv. The method has an average accuracy of 104% and precision of 13% relative standard deviation (RSD), with an instrument run time of 32 min. In addition, a link between canister cleanliness and ethylene oxide growth is observed, and potential mechanisms and cleaning strategies are addressed.

Residue Analysis of Organophosphorus and Organochlorine Pesticides in Fatty Matrices by Gas Chromatography Coupled with Electron-Capture Detection

2006 ◽  
Vol 61 (5-6) ◽  
pp. 341-346 ◽  
Author(s):  
Jae-Woo Park ◽  
A. M. Abd El-Aty ◽  
Myoung-Heon Lee ◽  
Sung-Ok Song ◽  
Jae-Han Shim
Keyword(s):  
Gas Chromatography ◽  
Electron Capture ◽  
Simple Procedure ◽  
Linear Regression Analysis ◽  
Residue Analysis ◽  
Electron Capture Detection ◽  
Relative Standard ◽  
Wide Range ◽  
Repeatability And Reproducibility

A multiresidue method for the simultaneous determination of 22 organochlorine (OCs) and organophosphorus (Ops) pesticides (including isomers and metabolites), representing a wide range of physicochemical properties, was developed in fatty matrices extracted from meat. Pesticides were extracted from samples with acetonitrile/n-hexane (v :v, 1:1). The analytical screening was performed by gas chromatography coupled with electron-capture detection (ECD). The identification of compounds was based on their retention time and on comparison of the primary and secondary ions. The optimized method was validated by determining accuracy (recovery percentages), precision (repeatability and reproducibility), and sensitivity (detection and quantitation limits) from analyses of samples fortified at 38 to 300 ng/g levels. Correlation coefficients for the 22 extracted pesticide standard curves (linear regression analysis, n = 3) ranged from 0.998 to 1.000. Recovery studies from 2 g samples fortified at 3 levels demonstrated that the GC-ECD method provides 64.4-96.0% recovery for all pesticides except 2,4′-DDE (44.6-50.4%), 4,4′-DDE (51.1-57.5%) and 2,4′-DDT (50.0-51.2%). Both repeatability and reproducibility relative standard deviation values were < 20% for all residues. Detection limits ranged from 0.31 to 1.27 ng/g and quantification limits were between 1.04 and 4.25 ng/g. The proposed analytical method may be used as a simple procedure in routine determinations of OCs and Ops in meat. It can also be applied to the determination of pesticide multi-residues in other animal products such as butter and milk.

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