scholarly journals Determination of Tetracycline and Fluoroquinolone Antibiotics at Trace Levels in Sludge and Soil

2015 ◽  
Vol 2015 ◽  
pp. 1-10 ◽  
Author(s):  
Marie-Virginie Salvia ◽  
Maëva Fieu ◽  
Emmanuelle Vulliet
Keyword(s):  
Analytical Method ◽  
Fluoroquinolone Antibiotics ◽  
Relative Standard ◽  
Standard Deviations ◽  
Spe Purification

This work describes the development of a sensitive analytical method to determine simultaneously traces of tetracycline and fluoroquinolone antibiotics in sludge and soil, based on PLE extraction, followed by SPE purification and finally an analysis by LC-MS/MS. Recoveries were greater than 87% in the case of fluoroquinolones and between 25.4 and 41.7% for tetracyclines. Low relative standard deviations (<15%) were obtained in both matrices. The limits of quantification were comprised between 1.1 and 4.6 ng/g and between 5 and 20 ng/g in soil and sludge, respectively. The method was then successfully applied to the analysis of the target antibiotics in sludge as well as soil that received spreading. The substances most frequently found and with the highest levels were fluoroquinolones with concentrations exceeding 1,000 ng/g in several samples of sludge and up to 16 ng/g in soil.

scholarly journals Multiwavelength Spectral Correction for the Simultaneous Determination of Cu(II), Fe(II), and Zn(II) with 1-(5-Bromo-2-Pyridylazo)-2-Naphthol-6-Sulfonic Acid

2001 ◽  
Vol 84 (1) ◽  
pp. 532-536 ◽  
Author(s):  
Hong-Wen Gao
Keyword(s):  
Simultaneous Determination ◽  
Analytical Method ◽  
Sulfonic Acid ◽  
Free Ligand ◽  
Spectral Correction ◽  
Relative Standard ◽  
Zn And Cu In ◽  
Matrix Formula ◽  
Standard Deviations

Abstract A new analytical method is described for the simultaneous determination of various components by multiwavelength spectrophotometry. Because of the influence of the free ligand and various complexes on spectrophotometric absorption, the spectral correction principle was used to establish the calculation matrix formula. The 3 sensitive reactions of Cu(II), Fe(II), and Zn(II), with 1-(5-bromo-2-pyridylazo)-2-naphthol-6-sulfonic acid were studied at pH 10.5. In analyses of fortified samples, the recoveries of Fe, Zn, and Cu were between 93.0 and 103%, 87.0 and 108%, and 92.5 and 108%, respectively; the relative standard deviations for 5 determinations of Fe, Zn, and Cu in unfortified ore were 3.6, 5.8, and 4.5%, respectively.

scholarly journals Simultaneous Determination of Nitroimidazoles and Quinolones in Honey by Modified QuEChERS and LC-MS/MS Analysis

2018 ◽  
Vol 2018 ◽  
pp. 1-12 ◽  
Author(s):  
Haiyan Lei ◽  
Jianbo Guo ◽  
Zhuo Lv ◽  
Xiaohong Zhu ◽  
Xiaofeng Xue ◽  
...  
Keyword(s):  
Recovery Rates ◽  
Inhibition Effect ◽  
Standard Curve ◽  
Modified Quechers ◽  
Relative Standard ◽  
Acacia Honey ◽  
The Matrix ◽  
Liquid Chromatography Tandem Mass ◽  
Standard Deviations

This study reports an analytical method for the determination of nitroimidazole and quinolones in honey using liquid chromatography-tandem mass spectrometry (LC-MS/MS). A modified QuEChERS methodology was used to extract the analytes and determine veterinary drugs in honey by LC-MS/MS. The linear regression was excellent at the concentration levels of 1–100 ng/mL in the solution standard curve and the matrix standard curve. The recovery rates of nitroimidazole and quinolones were 4.4% to 59.1% and 9.8% to 46.2% with relative standard deviations (RSDs) below 5.2% and the recovery rates of nitroimidazole and quinolones by the matrix standard curve ranged from 82.0% to 117.8% and 79% to 115.9% with relative standard deviations (RSDs) lower than 6.3% in acacia and jujube honey. The acacia and jujube honeys have stronger matrix inhibition effect to nitroimidazole and quinolones residue; the matrix inhibition effect of jujube honey is stronger than acacia honey. The matrix standard curve can calibrate matrix effect effectively. In this study, the detection method of antibiotics in honey can be applied to the actual sample. The results demonstrated that the modified QuEChERS method combined with LC-MS/MS is a rapid, high, sensitive method for the analysis of nitroimidazoles and quinolones residues in honey.

scholarly journals Determination of Ochratoxin A in Wine and Beer by Immunoaffinity Column Cleanup and Liquid Chromatographic Analysis with Fluorometric Detection: Collaborative Study

2001 ◽  
Vol 84 (6) ◽  
pp. 1818-1827 ◽  
Author(s):  
Angelo Visconti ◽  
Michelangelo Pascale ◽  
Gianluca Centonze ◽  
E Anklam ◽  
A M Betbeder ◽  
...  
Keyword(s):  
Ochratoxin A ◽  
Red Wine ◽  
Collaborative Study ◽  
White Wine ◽  
Fluorometric Detection ◽  
Immunoaffinity Column ◽  
Relative Standard ◽  
Standard Deviations ◽  
Liquid Chromatographic

Abstract The accuracy, repeatability, and reproducibility characteristics of a liquid chromatographic method for the determination of ochratoxin A (OTA) in white wine, red wine, and beer were established in a collaborative study involving 18 laboratories in 10 countries. Blind duplicates of blank, spiked, and naturally contaminated materials at levels ranging from ≤0.01 to 3.00 ng/mL were analyzed. Wine and beer samples were diluted with a solution containing polyethylene glycol and sodium hydrogen carbonate, and the diluted samples were filtered and cleaned up on an immunoaffinity column. OTA was eluted with methanol and quantified by reversed-phase liquid chromatography with fluorometric detection. Average recoveries from white wine, red wine, and beer ranged from 88.2 to 105.4% (at spiking levels ranging from 0.1 to 2.0 ng/mL), from 84.3 to 93.1% (at spiking levels ranging from 0.2 to 3.0 ng/mL), and from 87.0 to 95.0% (at spiking levels ranging from 0.2 to 1.5 ng/mL), respectively. Relative standard deviations for within-laboratory repeatability (RSDr) ranged from 6.6 to 10.8% for white wine, from 6.5 to 10.8% for red wine, and from 4.7 to 16.5% for beer. Relative standard deviations for between-laboratories reproducibility (RSDR) ranged from 13.1 to 15.9% for white wine, from 11.9 to 13.6% for red wine, and from 15.2 to 26.1% for beer. HORRAT values were ≤0.4 for the 3 matrixes.

Sulfuric Acid/Hydrogen Peroxide Digestion and Colorimetric Determination of Phosphorus in Meat and Meat Products: Collaborative Study

1991 ◽  
Vol 74 (1) ◽  
pp. 22-26 ◽  
Author(s):  
David K Christians ◽  
Thomas G Aspelund ◽  
Scott V Brayton ◽  
Larry L Roberts
Keyword(s):  
Hydrogen Peroxide ◽  
Sulfuric Acid ◽  
Collaborative Study ◽  
Meat Products ◽  
Colorimetric Determination ◽  
Pork Sausage ◽  
Relative Standard ◽  
Significant Difference ◽  
Standard Deviations

Abstract Seven laboratories participated In a collaborative study of a method for determination of phosphorus in meat and meat products. Samples are digested In sulfuric acid and hydrogen peroxide; digestion Is complete In approximately 10 mln. Phosphorus Is determined by colorimetric analysis of a dilute aliquot of the sample digest. The collaborators analyzed 3 sets of blind duplicate samples from each of 6 classes of meat (U.S. Department of Agriculture classifications): smoked ham, water-added ham, canned ham, pork sausage, cooked sausage, and hamburger. The calibration curve was linear over the range of standard solutions prepared (phosphorus levels from 0.05 to 1.00%); levels in the collaborative study samples ranged from 0.10 to 0.30%. Standard deviations for repeatability (sr) and reproducibility (sR) ranged from 0.004 to 0.012 and 0.007 to 0.014, respectively. Corresponding relative standard deviations (RSDr and RSDR, respectively) ranged from 1.70 to 7.28% and 3.50 to 9.87%. Six laboratories analyzed samples by both the proposed method and AOAC method 24.016 (14th Ed.). One laboratory reported results by the proposed method only. Statistical evaluations Indicated no significant difference between the 2 methods. The method has been adopted official first action by AOAC.

scholarly journals A Simplified Modification of the AOAC Official Method for Determination of Total Dietary Fiber Using Newly Developed Enzymes: Preliminary Interlaboratory Study

2007 ◽  
Vol 90 (1) ◽  
pp. 225-237 ◽  
Author(s):  
Kenichiro Kanaya ◽  
Shusaku Tada ◽  
Bunpei Mori ◽  
Rie Takahashi ◽  
Sachie Ikegami ◽  
...  
Keyword(s):  
Dietary Fiber ◽  
Enzymatic Digestion ◽  
Interlaboratory Study ◽  
Total Dietary Fiber ◽  
Stabilizing Agents ◽  
Modified Method ◽  
Relative Standard ◽  
Aoac Method ◽  
Standard Deviations

Abstract A preliminary interlaboratory study was conducted to evaluate the validity of the modified AOAC method for determination of total dietary fiber by Tada and Innami, in which the 3-step enzymatic digestion process in AOAC Method 991.43 is modified to a 2-step process without pH adjustment. Total dietary fiber contents in 8 representative foodstuffs were measured using both the original AOAC Method 991.43 and the modified method in 6 research facilities in Japan. Repeatability relative standard deviations, reproducibility relative standard deviations, and Horwitz ratio values from the modified method were equivalent to those from AOAC Method 991.43, except in the rice sample. However, this exceptional case shown in the modified method was entirely dissolved by the addition of α-amylase stabilizing agents. The modified method, which shortens the process of enzymatic digestion from 3 to 2 steps and in which only reaction temperature is adjusted under the same pH, was found not only to give accurate values comparable to the original method, but also to substantially reduce the labor required by the laboratory staff in the process of routine analysis. This study revealed that the validity of the modified method was further ensured by adding α-amylase stabilizing agents to the reaction system.

Generic Combustion Method for Determination of Crude Protein in Feeds: Collaborative Study

1989 ◽  
Vol 72 (5) ◽  
pp. 770-774 ◽  
Author(s):  
Rose A Sweeney
Keyword(s):  
Crude Protein ◽  
Collaborative Study ◽  
Combustion Method ◽  
Performance Requirements ◽  
General Terms ◽  
Relative Standard ◽  
Kjeldahl Method ◽  
Standard Deviations ◽  
And Performance

Abstract Nine laboratories participated in a collaborative study on determination of crude protein in animal feeds to compare a generically described combustion method with the AOAC mercury catalyst Kjeldahl method (7.015). The combustion method was written in general terms of method principle, apparatus specifications, and performance requirements. The sample set comprised closely matched pairs of feed ingredients and mixed products ranging from 10 to 90% protein. Ten pairs ground to 0.5 mm were the focus of the study; 4 pairs were ground to 1.0 mm for comparison. Nicotinic acid and lysine monohydrochloride were included as standards. Collaborators were instructed to report their results for performance checks using materials supplied. Only one laboratory failed to meet the proposed limits. Seven laboratories used the LECO Model FP-228 analyzer and 2 used the LECO CHN 600 analyzer. For the 0.5 mm pairs, repeatability standard deviations (sr) ranged from 0.09 to 0.58 for the Kjeldahl method and from 0.14 to 0.33 for the combustion method, with a pooled sr value of 0.28 and relative standard deviation (RSDr) of 0.59%. Reproducibility standard deviations (SR) ranged from 0.23 to 0.86 (Kjeldahl) and from 0.30 to 0.61 (combustion), with a pooled sR value of 0.52 and RSDR of 1.10%. Grand means for the samples ground to 0.5 mm were 47.65% protein by the combustion method and 47.41% protein by the Kjeldahl method. For samples ground to 1.0 mm, corresponding values were 31.82 and 31.50% protein. The generic combustion method has been approved interim official first action.

scholarly journals Determination of Arsenic, Cadmium, Mercury, and Lead by Inductively Coupled Plasma/Mass Spectrometry in Foods after Pressure Digestion: NMKL Interlaboratory Study

2007 ◽  
Vol 90 (3) ◽  
pp. 844-856 ◽  
Author(s):  
Kaare Julshamn ◽  
Amund Maage ◽  
Hilde Skaar Norli ◽  
Karl H Grobecker ◽  
Lars Jorhem ◽  
...  
Keyword(s):  
Mass Spectrometry ◽  
Inductively Coupled Plasma ◽  
Method Performance ◽  
Inductively Coupled ◽  
Icp Ms ◽  
Relative Standard ◽  
Limit Of Quantitation ◽  
Plasma Mass Spectrometry ◽  
Standard Deviations

Abstract Thirteen laboratories participated in an interlaboratory method performance (collaborative) study on a method for the determination of arsenic, cadmium, mercury, and lead by inductively coupled plasma/mass spectrometry (ICP/MS) after pressure digestion including the microwave heating technique. Prior to the study, the laboratories were able to practice on samples with defined element levels (pretrial test). The method was tested on a total of 7 foodstuffs: carrot puree, fish muscle, mushroom, graham flour, simulated diet, scampi, and mussel powder. The elemental concentrations in mg/kg dry matter (dm) ranged from 0.0621.4 for As, 0.0328.3 for Cd, 0.040.6 for Hg, and 0.012.4 for Pb. The materials used in the study were presented to the participants as blind duplicates, and the participants were asked to perform single determinations on each sample. The repeatability relative standard deviations (RSDr) for As ranged from 3.8 to 24%, for Cd from 2.6 to 6.9%, for Hg from 4.8 to 8.3%, and for Pb from 2.9 to 27%. The reproducibility relative standard deviations (RSDR) for As ranged from 9.0 to 28%, for Cd from 2.8 to 18%, for Hg from 9.9 to 24%, and for Pb from 8.0 to 50%. The HorRat values were less than 1.5 for all test samples, except for the determination of Pb in wheat flour at a level close to the limit of quantitation (0.01 mg/kg dm). The study showed that the ICP/MS method is satisfactory as a standard method for elemental determinations in foodstuffs.

Optimization of an Aqueous Two-Phase System for the Determination of Trace Ethyl Carbamate in Red Wine

2019 ◽  
Vol 82 (8) ◽  
pp. 1377-1383 ◽  
Author(s):  
LIJUAN MA ◽  
WENZHE TONG ◽  
LIPING DU ◽  
SHIYONG HUANG ◽  
JINYAN WEI ◽  
...  
Keyword(s):  
Quantitative Determination ◽  
Red Wine ◽  
Ethyl Carbamate ◽  
Phase System ◽  
Extraction Temperature ◽  
Two Phase ◽  
Aqueous Two Phase System ◽  
Relative Standard ◽  
Standard Deviations

ABSTRACT In this study, a novel method using gas chromatography–mass spectrometry coupled with ethanol and K2HPO4 aqueous two-phase system (ATPS) was established for the quantitative determination of trace ethyl carbamate (EC) in red wine. The parameters that influence EC extraction in an aqueous two-phase system, including extraction temperature, time, pH, and ethanol concentration, were optimized. Method validation results indicated that the regression coefficient of the proposed method was 0.9979 in the linear range of 10 to 100 μg/L, and the limits of detection and quantification were 2.8 and 9.2 μg/L, respectively. Four red wine samples made from different grape varieties were processed by the proposed method for the repeatability verification, and EC concentrations were between 15.8 and 37.3 μg/L, with the relative standard deviations ranging from 3.5 to 6.6%. Results of the precision assay showed the average recovery of EC in red wine at 95.4 to 107.1%, with the relative standard deviations ranging from 1.4 to 6.2%. This method proved to be simple and reliable for quantitative determination of trace EC in red wine and would give guidance for quality monitoring of various red wines in the production process.

Liquid Chromatographic Method for Determination of Iodine in Milk: Collaborative Study

1993 ◽  
Vol 76 (4) ◽  
pp. 711-719 ◽  
Author(s):  
David Sertl ◽  
William Malone ◽  
◽  
P Beljaars ◽  
C Blake ◽  
...  
Keyword(s):  
Membrane Filter ◽  
Collaborative Study ◽  
Reversed Phase ◽  
Powdered Milk ◽  
Insoluble Material ◽  
Relative Standard ◽  
Repeatability And Reproducibility ◽  
Standard Deviations ◽  
Liquid Chromatographic

Abstract Nine laboratories participated in an AOAC International/ International Dairy Federation collaborative study on a liquid chromatographic (LC) method for determination of iodine in milk. Liquid milk is passed through a 25 000 MW membrane filter to remove protein and insoluble material. Iodine (in the form of iodide) in the clear filtrate is separated by reversed-phase ion-pair LC and is detected electrochemically. Participants analyzed 2 commercial pasteurized whole milks and 5 nonfat dry milk powders in blind duplicate. Each sample was tested in duplicate on 2 days. Repeatability and reproducibility standard deviations (sr and SR, respectively) and repeatability and reproducibility relative standard deviations (RSDr and RSDR, respectively) for determinations of iodine in whole milk (mean recovery, 86.7%) were as follows: sr, 22 μg/L; SR, 22 μg/L; RSDr, 8.2%; and RSDR, 8.3%. For powdered milk (mean recovery, 91 %), the values were as follows: sr, 0.14 μg/g; SR, 0.22 μg/g; RSDr, 9.0%; and RSDR, 12.7%. The method was adopted first action by AOAC International.

X-Ray Absorption-Edge Determination of Cobalt in Complex Mixtures*

1961 ◽  
Vol 5 ◽  
pp. 379-388
Author(s):  
E.A. Hakkila ◽  
G.R. Waterbury
Keyword(s):  
Nitric Acid ◽  
Absorption Edge ◽  
Path Length ◽  
Construction Materials ◽  
X Ray ◽  
Relative Standard ◽  
Standard Deviations ◽  
Low X ◽  
X Ray Absorption

AbstractThe application of the X-ray absorption-edge technique was extended to the determination of cobalt in aqueous and alcoholic solutions containing a wide variety of impurity elements. In the procedure developed, secondary radiation from a 50% copper-nickel alloy is passed through an absorption cell filled alternately with the solvent and the sample solution. The transmitted Intensities of the Kα lines for copper and nickel are measured, and the concentration of cobalt is determined using accepted absorption principles. The K absorption edge for cobalt occurs at 1.604 A, restricting cell construction materials and solvents to those containing light elements with low X-ray absorption characteristics and also limiting the path length of the cell.Cells of 0.16- and 0.34-cm path length were used in the analysis of aqueous and alcoholic solutions, respectively. With the 0.16-cm path-length cell, relative standard deviations of 4.6 to 0.5% were obtained for cobalt concentrations ranging from 1.00 to 10.00 mg/ml for known aqueous solutions that contain various known concentrations of nitric acid. With the longer path-length cell, relative standard deviations from 1.8 to 0.46% were obtained for cobalt concentrations in the same range in known alcoholic solutions containing various known concentrations of nitric acid. The standard deviation of determining the blank is 0.043 mg of cobalt per milliliter for the 0.16-cm cell and 0.016 mg of cobalt per milliliter for the longer cell.A Norelco X-ray spectrograph with a three-position head was used in these analyses. Less than 5 min is required to convert this instrument from normal fluorescence operation to absorption-edge analysis. Approximately 15 to 20 analyses can be performed daily.

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