scholarly journals Preparation of an immunoaffinity chromatography column for chloramphenicol binding

2016 ◽  
Vol 19 (4) ◽  
pp. 14-23
Author(s):  
Thinh Duc Nguyen ◽  
Thu Thi Nguyet Nguyen ◽  
Diem Ngoc Duong ◽  
Son Pham Ngoc Chu ◽  
Thuoc Linh Tran
Keyword(s):  
Limit Of Detection ◽  
Immunoaffinity Chromatography ◽  
Loading Capacity ◽  
Tandem Mass ◽  
Rabbit Antibody ◽  
Limit Of Quantification ◽  
Chromatography Tandem Mass Spectrometry ◽  
Liquid Chromatography Tandem Mass ◽  
Chromatography Columns ◽  
Cap Analysis

Anti-chloramphenicol rabbit antibody was covalently bound to Sepharose CL 4B-CNBr gel at 5, 10 and 15 mg antibody per mL gel and was fed into columns to prepare three respective immunoaffinity chromatography columns for chloramphenicol (CAP) binding. Examination of CAP-binding efficiency of these columns being fed with 0.5, 1 and 10 ng CAP showed that the column with 10 mg antibody per ml gel (IAC-CAP-10 column) could bind more than 90 % of the CAP amount having been fed into the column at all three examined CAP amounts. This IAC-CAP-10 column showed a coefficient of variants (CV) between columns upon CAP binding of 5.18 % for 1 ng fed CAP and 1.98 % for 10 ng, respectively, a loading capacity of 153,37 ± 10,32 ng CAP, stable CAP-binding performance during at least 2 years of preservation at 4 °C. The coupling of this IAC-CAP-10 column with liquid chromatography - tandem mass spectrometry LC MS/MS could make CAP analysis become possible with a limit of detection LOD of 0.033 ng and a limit of quantification LOQ of 0.101 ng. The column could also bind to the other two phenicol antibiotics: florfenicol and thiamphenicol with a binding efficiency of 90.73 % for florfenicol and 84.29 % for thiamphenicol.

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.

scholarly journals Determination of Polyphenol Components of Korean Prostrate Spurge (Euphorbia supina) by Using Liquid Chromatography—Tandem Mass Spectrometry: Overall Contribution to Antioxidant Activity

2014 ◽  
Vol 2014 ◽  
pp. 1-8 ◽  
Author(s):  
Yi Song ◽  
Sung Woo Jeong ◽  
Won Sup Lee ◽  
Semin Park ◽  
Yun-Hi Kim ◽  
...  
Keyword(s):  
Mass Spectrometry ◽  
Liquid Chromatography ◽  
Tandem Mass Spectrometry ◽  
Limit Of Detection ◽  
Antioxidant Activities ◽  
Reducing Power ◽  
Tandem Mass ◽  
Limit Of Quantification ◽  
Chromatography Tandem Mass Spectrometry ◽  
Liquid Chromatography Tandem Mass

The Korean prostrate spurgeEuphorbia supinais a weed that has been used in folk medicine in Korea against a variety of diseases. Nine polyphenols were characterized for this plant by using high-performance liquid chromatography-tandem mass spectrometry (HPLC-MS/MS) and the results were compared with the literature data. The individual components were validated using the calibration curves of structurally related external standards and quantified for the first time by using the validated method. Correlation coefficients (r2) were >0.9907. The limit of detection and limit of quantification of the method were >0.028 mg/L and 0.094 mg/L, respectively. Recoveries measured at 50 mg/L and 100 mg/L were 76.1–102.8% and 85.2–98.6%, respectively. The total amount of the identified polyphenols was 3352.9 ± 2.8 mg/kg fresh plant. Quercetin and kaempferol derivatives formed 84.8% of the total polyphenols. The antioxidant activities of the flavonoids were evaluated in terms of 1,1-diphenyl-2-picrylhydrazyl and 2,2′-azinobis(3-ethylbenzothiazoline-6-sulfonic acid) radical cation-scavenging activity, and the reducing power showed a dose-dependent increase. Cell viability was effectively suppressed at polyphenol mixture concentrations >250 mg/L.

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 A novel high-throughput assay for the measurement of salivary progesterone by liquid chromatography tandem mass spectrometry

2018 ◽  
Vol 56 (1) ◽  
pp. 64-71 ◽  
Author(s):  
Lina Schiffer ◽  
Joanne E Adaway ◽  
Elizabeth S Baranowski ◽  
Wiebke Arlt ◽  
Brian G Keevil
Keyword(s):  
Mass Spectrometry ◽  
Liquid Chromatography ◽  
Menstrual Cycle ◽  
Tandem Mass Spectrometry ◽  
High Throughput ◽  
Large Set ◽  
Tandem Mass ◽  
Limit Of Quantification ◽  
Chromatography Tandem Mass Spectrometry ◽  
Liquid Chromatography Tandem Mass

Background Liquid chromatography tandem mass spectrometry (LC-MS/MS) enables specific and sensitive quantification of steroids with a high throughput. Saliva sampling is advantageous for multisample profiling over longer periods of time, as it is non-invasive, cheap, can be carried out at home and does not require the attendance of clinical personnel. We developed a rapid LC-MS/MS for the measurement of salivary progesterone, frequently assessed as ovulation marker in patients desiring fertility. Methods Samples (300 μL) were prepared by supported liquid extraction using dichloromethane and were reconstituted in 40% methanol. Chromatography was performed using a C8 column with a water/methanol gradient containing 0.1% formic acid and 2 mmol/L ammonium acetate. Quantification was performed with a Waters TQ-S mass spectrometer. Results Total run time was 5.5 min. The lower limit of quantification was 20 pmol/L (1.2 fmol on column). Inter- and intra-assay comparison showed coefficients of variation and bias between measured and nominal concentrations of less than 11%. Mean recovery was 91%. Interference with a large set of natural and synthetic steroids was excluded. The assay was successfully applied to measure progesterone variation during the menstrual cycle ( n = 9) and diurnal variations during luteal phase ( n = 7) in regularly cycling women. Discussion We present a novel LC-MS/MS assay for the determination of salivary progesterone with high-throughput potential. The applicability of the assay for progesterone profiling during the menstrual cycle is demonstrated.

scholarly journals Sample Multiplexing: Increased Throughput for Quantification of Total Testosterone in Serum by Liquid Chromatography-Tandem Mass Spectrometry

2020 ◽  
Vol 66 (9) ◽  
pp. 1181-1189 ◽  
Author(s):  
Julia D Colletti ◽  
Mildred M Redor-Goldman ◽  
Agustin E Pomperada ◽  
Amit K Ghoshal ◽  
William W Wu ◽  
...  
Keyword(s):  
Mass Spectrometry ◽  
Liquid Chromatography ◽  
Tandem Mass Spectrometry ◽  
Method Comparison ◽  
Total Testosterone ◽  
Tandem Mass ◽  
Limit Of Quantification ◽  
Chromatography Tandem Mass Spectrometry ◽  
Deming Regression ◽  
Liquid Chromatography Tandem Mass

Abstract BACKGROUND For high-volume assays, optimizing throughput reduces test cost and turn-around time. One approach for liquid chromatography-tandem mass spectrometry (LC-MS/MS) assays is sample multiplexing, wherein the analyte of interest is derivatized in different specimens with reagents of different molecular weight (differential mass tagging). Specimens can then be combined and simultaneously analyzed within a single injection to improve throughput. Here we developed and validated a quantitative, sample-multiplexed LC-MS/MS assay for serum total testosterone (TT) based on this approach. METHODS For the sample-multiplexed assay, calibrators, controls, and patient specimens were first extracted separately. After mass tagging with either methoxyamine or hydroxylamine, they were combined and injected into the LC-MS/MS system. To evaluate assay performance, we determined limit of quantification (LOQ), linearity, recovery, and imprecision. A method-comparison study was also performed, comparing the new assay with the standard LC-MS/MS assay in 1574 patient specimens. RESULTS The method was linear from 2.5 to 2000 ng/dL, with accuracies from 93% to 104% for both derivatives. An LOQ of 1.0 ng/dL was achieved. Intra-assay and total CVs across 4 quality control concentrations were less than 10%. The assay demonstrated good agreement (Deming regression, 1.03x + 6.07) with the standard LC-MS/MS assay for the patient specimens tested (TT, 3 to 4862 ng/dL). CONCLUSION Sample multiplexing by differential mass tagging of TT increases LC-MS/MS throughput 2-fold without compromising analytical accuracy and sensitivity.

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