scholarly journals Quantitative LC/MS-MS Determination of Sulfonamides and Some Other Antibiotics in Honey

2002 ◽  
Vol 85 (4) ◽  
pp. 853-860 ◽  
Author(s):  
Anton Kaufmann ◽  
Sven Roth ◽  
Bianca Ryser ◽  
Mirjam Widmer ◽  
Dominik Guggisberg
Keyword(s):  
Mass Spectrometry ◽  
Liquid Chromatography ◽  
Tandem Mass Spectrometry ◽  
Rapid Method ◽  
Limit Of Detection ◽  
Tandem Mass ◽  
Chromatography Tandem Mass Spectrometry ◽  
Liquid Chromatography Tandem Mass

Abstract A simple and rapid method was developed for the determination of 20 antibiotics (sulfonamides, tetracyclines, and flumequine) in honey by liquid chromatography tandem mass spectrometry. The proposed method is sensitive (limit of detection 0.5 to 10 ppb for the various antibiotics) and selective. A hydrolysis step ensures the liberation of sugar-bound sulfonamides. The approach has been used to analyze some 300 honey samples. A number of them were found to have exceeded the Swiss limit of 50 ppb.

scholarly journals Multi-Class Determination of 64 Illicit Compounds in Dietary Supplements Using Liquid Chromatography–Tandem Mass Spectrometry

Molecules ◽  
2020 ◽  
Vol 25 (19) ◽  
pp. 4399
Author(s):  
Dasom Shin ◽  
Hui-Seung Kang ◽  
Hyungsoo Kim ◽  
Guiim Moon
Keyword(s):  
Mass Spectrometry ◽  
Liquid Chromatography ◽  
Tandem Mass Spectrometry ◽  
Dietary Supplements ◽  
Limit Of Detection ◽  
Tandem Mass ◽  
Chromatography Tandem Mass Spectrometry ◽  
Relative Standard ◽  
Liquid Chromatography Tandem Mass

In this work, liquid chromatography–tandem mass spectrometry (LC-MS/MS) method was developed and validated for screening and confirmation of 64 illicit compounds in dietary supplements. The target compounds were illegally used pharmaceutical drugs, prohibited compounds, and not authorized ingredients for different therapeutics (sexual enhancement, weight loss, muscular strengthening, and relaxing products). The validation procedure was performed to evaluate selectivity, linearity, limit of detection (LOD), limit of quantification (LOQ), accuracy, and precision according to the Association of Official Analytical Chemists guidelines. The linearity was >0.98 in the range of 0.5–200 µg L−1. The LOQs were in the range 1–10 µg kg−1 for all target compounds. The accuracy (expressed as recovery) was 78.5–114%. The precision (expressed as the relative standard deviation) was below 9.15%. The developed method was applied for the determination of illicit compounds in dietary supplements collected from websites. As a result, the total detection rate was 13.5% (27 samples detected in 200 samples). The concentrations of detected samples ranged from 0.51 to 226 mg g−1. The proposed methodology is suitable for monitoring the adulteration of illicit compounds in dietary supplements.

scholarly journals Determination of Four Nitroimidazoles in Poultry and Swine Muscle and Eggs by Liquid Chromatography/Tandem Mass Spectrometry

2006 ◽  
Vol 89 (1) ◽  
pp. 94-99 ◽  
Author(s):  
Xi Xia ◽  
Xiaowei Li ◽  
Jianzhong Shen ◽  
Suxia Zhang ◽  
Shuangyang Ding ◽  
...  
Keyword(s):  
Mass Spectrometry ◽  
Liquid Chromatography ◽  
Tandem Mass Spectrometry ◽  
Rapid Method ◽  
Organic Phase ◽  
Tandem Mass ◽  
Chromatography Tandem Mass Spectrometry ◽  
Liquid Chromatography Tandem Mass ◽  
Detection Capabilities

Abstract A rapid method is presented for the determination of 4 nitroimidazoles in poultry and swine muscle and eggs by liquid chromatographyelectrospray ionizationtandem mass spectrometry (LCESIMSMS). Samples were extracted with acetonitrile, then evaporated the organic phase. After filtration, the extract was directly injected into the LCESIMSMS system. The LC separation was made on a C8 column by applying a gradient composed of water and acetonitrile. Overall average recoveries ranged from 5086 for egg, 66115 for poultry muscle, and 79111 for swine muscle. The decision limits ranged from 0.05-0.25 μgkg for egg, 0.07-0.27 μgkg for poultry muscle, and 0.07-0.26 μgkg for swine muscle; and detection capabilities ranged from 0.510.68 gkg for egg, 0.41-0.75 μgkg for poultry muscle, and 0.53-0.78 μgkg for swine muscle.

scholarly journals Determination of Cyclamate in Foods by Ultraperformance Liquid Chromatography/Tandem Mass Spectrometry

2008 ◽  
Vol 91 (5) ◽  
pp. 1095-1102 ◽  
Author(s):  
Robert Sheridan ◽  
Thomas King
Keyword(s):  
Mass Spectrometry ◽  
Liquid Chromatography ◽  
Sample Preparation ◽  
Tandem Mass Spectrometry ◽  
Limit Of Detection ◽  
Tandem Mass ◽  
Chromatography Tandem Mass Spectrometry ◽  
Limit Of Quantitation ◽  
Liquid Chromatography Tandem Mass

Abstract A highly sensitive and selective method that requires minimal sample preparation was developed for the confirmation and quantitation of cyclamate in a variety of foods by high-performance liquid chromatography/tandem mass spectrometry (HPLC/MS/MS). Sample preparation consisted of homogenization followed by extraction and dilution of cyclamate with water. HPLC separation was achieved using a bridged ethyl hybrid C18 high-pressure column with a mobile phase consisting of 0.15 acetic acid and methanol. Under electrospray ionization negative conditions, quantitation was achieved by monitoring the fragment m/z 79.7 while also collecting parent ion m/z 177.9. Two food matrixes, diet soda and jelly, were subjected to a validation procedure in order to evaluate the applicability of the method. The cyclamate limit of detection for both matrixes was determined to be 0.050 g/g with a limit of quantitation of 0.150 g/g. The correlation coefficient of the calibration curves was >0.9998 from 0.0005 to 0.100 g/mL. The method has been used for the determination of cyclamate in several foods and the results are presented.

scholarly journals Liquid Chromatography-Tandem Mass Spectrometry Method for the Determination of Vardenafil and Its Application of Bioequivalence

2021 ◽  
Vol 2021 ◽  
pp. 1-10
Author(s):  
Kok Zheng Gan ◽  
Riyanto Teguh Widodo ◽  
Zamri Chik ◽  
Lay Kek Teh ◽  
Mohd Salleh Rofiee ◽  
...  
Keyword(s):  
Mass Spectrometry ◽  
Liquid Chromatography ◽  
Tandem Mass Spectrometry ◽  
Limit Of Detection ◽  
Internal Standard ◽  
Tandem Mass ◽  
Rabbit Plasma ◽  
Chromatography Tandem Mass Spectrometry ◽  
Liquid Chromatography Tandem Mass

A simple, rapid, and sensitive method of liquid chromatography-tandem mass spectrometry (LC/MS/MS) method was developed and validated for the determination of vardenafil in rabbit plasma. A simple protein precipitation method with ice-cold acetonitrile was used for plasma extraction. The mass transitions m/z 489⟶151 and m/z 390⟶169 were used to measure vardenafil and tadalafil (internal standard), respectively, with a total assay run time of 6 min. The limit of detection was 0.2 ng/mL. The assay was reproducible with intra-assay and interassay precision ranging 1.17%–9.17% and 1.31%–5.86%, respectively. There was also good intra-assay and interassay accuracy between 89.3%–105.3% and 94%–102% of the expected value, respectively. The linearity range was 0.5–60 ng/mL in rabbit plasma ( r 2  ≥ 0.99). The measured AUC from 0 to 24 h AUC 0 − 24 t for the test and reference formulations were 174.38 ± 95.91 and 176.45 ± 76.88, respectively. For the test, C max and T max were 75.36 ± 59.53 ng/mL and 1.42 ± 0.19 h, whereas, for the reference, these were 58.22 ± 36.11 ng/mL and 2.04 ± 0.33 h, respectively. The test formulation achieved a slightly lower AUC 0 − 24 t value ( p  > 0.05), higher C max values ( p  > 0.05), faster T max ( p  < 0.05), and almost equal bioavailability compared with the reference formulation.

Determination of aflatoxins in commercial nuts and nut products using liquid chromatography tandem mass spectrometry

2011 ◽  
Vol 4 (2) ◽  
pp. 119-127 ◽  
Author(s):  
Y. Leong ◽  
N. Ismail ◽  
A. Latiff ◽  
N. Manaf ◽  
A. Rosma
Keyword(s):  
Mass Spectrometry ◽  
Liquid Chromatography ◽  
Tandem Mass Spectrometry ◽  
Limit Of Detection ◽  
Natural Occurrence ◽  
Tandem Mass ◽  
Chromatography Tandem Mass Spectrometry ◽  
Liquid Chromatography Tandem Mass ◽  
Aflatoxin B

A rapid and sensitive confirmatory analytical method for determination of aflatoxins in nuts and their products using liquid chromatography tandem mass spectrometry has been developed and validated. All four aflatoxins of interest (B1, B2, G1 and G2) were quantified using aflatoxin M1 as the internal standard. Samples were extracted using methanol/water (60:40, v/v) and cleaned-up with immunoaffinity column. Limit of detection ranged between 0.10 and 0.30 µg/kg. Recovery rates were between 76 and 105% for all analytes. For further validation, a reference material for contaminated peanut has been used for quality assurance measures to check the accuracy and precision. The method was successfully applied to determine the natural occurrence of aflatoxins in 128 nut samples marketed in Penang, Malaysia. More than half of the samples (57.0%) were positive and 13.3% were found to be non-compliant with the European Commission regulations permitted maximum level of 2 µg/kg for aflatoxin B1. The contamination levels ranged from 0.40 to 221.61 µg/kg for aflatoxin B1 and 0.33 to 273.63 µg/kg for total aflatoxins.

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