scholarly journals UPLC-MS/MS Method for Simultaneous Determination of Three Major Metabolites of Mequindox in Holothurian

2018 ◽  
Vol 2018 ◽  
pp. 1-7 ◽  
Author(s):  
Huihui Liu ◽  
Chuanbo Ren ◽  
Dianfeng Han ◽  
Hui Huang ◽  
Rongjie Zou ◽  
...  
Keyword(s):  
Mass Spectrometry ◽  
Limit Of Detection ◽  
Tandem Mass ◽  
Limit Of Quantification ◽  
Chromatography Tandem Mass Spectrometry ◽  
Target Analytes ◽  
Liquid Chromatography Tandem Mass ◽  
Positive Rate ◽  
Ultrasound Assisted

This study developed an ultraperformance liquid chromatography tandem mass spectrometry (UPLC-MS/MS) method for the detection of three major metabolites of mequindox, including 3-methyl-quinoxaline-2-carboxylic acid, 1-desoxymequindox, and 1,4-bisdesoxymequindox (MQCA, 1-DMEQ, and BDMEQ), in holothurian. Target analytes were simplified with ultrasound-assisted acidolysis extracted without complicated enzymolysis steps. After that, each sample was centrifuged and purified by an Oasis MAX cartridge. Then, the processed samples were separated and monitored by UPLC-MS/MS. This developed method has been validated according to FDA criteria. At fortified levels of 2, 10, and 20 μg/kg, recoveries ranged from 82.5% to 93.5% with the intraday RSD less than 7.27% and interday RSD less than 11.8%. The limit of detection (LOD) of all the three metabolites ranged from 0.21 to 0.48 μg/kg, while the limit of quantification (LOQ) ranged from 0.79 to 1.59 μg/kg. On application to commercial samples, 14 of 20 samples were detected positive for the three target analytes, with positive rate at 70 percentage. The result indicated that this method was specific, sensitive, and suitable for the quantification and conformation of the three major metabolites of MEQ in holothurian.

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 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.

Determination of steroid hormones in sediments based on quick, easy, cheap, effective, rugged, and safe (modified-QuEChERS) extraction followed by liquid chromatography-tandem mass spectrometry (LC-MS/MS)

2015 ◽  
Vol 7 (22) ◽  
pp. 9577-9586 ◽  
Author(s):  
Julien Camilleri ◽  
Emmanuelle Vulliet
Keyword(s):  
Mass Spectrometry ◽  
Liquid Chromatography ◽  
Tandem Mass Spectrometry ◽  
Steroid Hormones ◽  
Tandem Mass ◽  
Modified Quechers ◽  
Chromatography Tandem Mass Spectrometry ◽  
Target Analytes ◽  
Liquid Chromatography Tandem Mass

The method enables the determination of the target analytes with limits of detection comprised between 0.03 and 0.2 ng g¬1and limits of quantification comprised between 0.1 and 0.6 ng g¬1.

Determination of 21 plant growth regulators in tomatoes using an improved ultrasound-assisted QuEChERS technique combined with a liquid chromatography tandem mass spectrometry method

2016 ◽  
Vol 8 (24) ◽  
pp. 4808-4815 ◽  
Author(s):  
Ren Shuiying ◽  
Wan Hongfei ◽  
Feng Shun ◽  
Wang Jide ◽  
Lu Yi
Keyword(s):  
Mass Spectrometry ◽  
Liquid Chromatography ◽  
Plant Growth ◽  
Tandem Mass ◽  
Spectrometry Method ◽  
Modified Quechers ◽  
Chromatography Tandem Mass Spectrometry ◽  
Liquid Chromatography Tandem Mass ◽  
Ultrasound Assisted

Simultaneous determination of 21 PGR in tomatoes through a modified QuEChERS technique coupled with LC-MS/MS.

scholarly journals Quantification of Degradation Products Formed during Heat Sterilization of Glucose Solutions by LC-MS/MS: Impact of Autoclaving Temperature and Duration on Degradation

2021 ◽  
Vol 14 (11) ◽  
pp. 1121
Author(s):  
Sarah Leitzen ◽  
Matthias Vogel ◽  
Michael Steffens ◽  
Thomas Zapf ◽  
Christa Elisabeth Müller ◽  
...  
Keyword(s):  
Mass Spectrometry ◽  
High Performance ◽  
Limit Of Detection ◽  
Degradation Products ◽  
High Reactivity ◽  
Tandem Mass ◽  
Specific Time ◽  
Limit Of Quantification ◽  
Chromatography Tandem Mass Spectrometry ◽  
Liquid Chromatography Tandem Mass

Heat sterilization of glucose solutions can lead to the formation of various glucose degradation products (GDPs) due to oxidation, hydrolysis, and dehydration. GDPs can have toxic effects after parenteral administration due to their high reactivity. In this study, the application of the F0 concept to modify specific time/temperature models during heat sterilization and their influence on the formation of GDPs in parenteral glucose solutions was investigated using high-performance liquid chromatography-tandem mass spectrometry (LC-MS/MS). Glucose solutions (10%, w/v) were autoclaved at 111 °C, 116 °C, and 121 °C for different durations. The GDPs glyoxal, methylglyoxal, glucosone, 3-deoxyglucosone/3-deoxygalactosone, 3,4-dideoxyglucosone-3-ene, and 5-hydroxymethylfurfural were quantified after derivatization with o-phenylenediamine by an optimized LC-MS/MS method. For all GDPs, the limit of detection was <0.078 μg/mL, and the limit of quantification was <0.236 μg/mL. The autoclaving time of 121 °C and 15 min resulted in the lowest levels of 3-DG/3-DGal and 5-HMF, but in the highest levels of GO and 2-KDG. The proposed LC-MS/MS method is rapid and sensitive. So far, only 5-HMF concentrations are limited by the regulatory authorities. Our results suggest reconsidering the impurity limits of various GDPs, especially the more toxic ones such as GO and MGO, by the Pharmacopoeias.

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