Detection of Antimicrobial Residues in Poultry Litter: Monitoring a Risk through a Selective and Sensitive HPLC–MS/MS Method

Tetracyclines, sulphonamides, and quinolones are families of antimicrobials (AMs) widely used in the poultry industry and can excrete up to 90% of AMs administrated, which accumulate in poultry litter. Worryingly, poultry litter is widely used as an agriculture fertilizer, contributing to the spread AMs residues in the environment. The aim of this research was to develop a method that could simultaneously identify and quantify three AMs families in poultry litter by high-performance liquid chromatography–tandem mass spectrometry (HPLC–MS/MS). Samples of AMs free poultry litter were used to validate the method according to 657/2002/EC and VICH GL49. Results indicate that limit of detection (LOD) ranged from 8.95 to 20.86 μg kg−1, while limits of quantitation (LOQ) values were between 26.85 and 62.58 µg kg−1 of tetracycline, 4-epi-tetracycline, oxytetracycline, 4-epi-oxytetracycline, enrofloxacin, ciprofloxacin, flumequine, sulfachloropyridazine, and sulfadiazine. Recoveries obtained ranged from 93 to 108%. The analysis of field samples obtained from seven commercial poultry flocks confirmed the adequacy of the method since it detected means concentrations ranging from 20 to 10,364 μg kg−1. This provides us an accurate and reliable tool to monitor AMs residues in poultry litter and control its use as agricultural fertilizer.

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

Pharmaceuticals ◽

10.3390/ph14111121 ◽

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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Simultaneous Analysis of Seven Neonicotinoids in Commercial Milk Samples Using an UHPLC-MS/MS Method

Applied Sciences ◽

10.3390/app10196775 ◽

2020 ◽

Vol 10 (19) ◽

pp. 6775

Author(s):

Yu-Fang Huang ◽

Yi-Min Huang ◽

Hsin-Jui Lee

Keyword(s):

High Performance ◽

Limit Of Detection ◽

Liquid Extraction ◽

Simultaneous Analysis ◽

Detection Range ◽

Milk Samples ◽

Liquid Liquid Extraction ◽

Chromatography Tandem Mass Spectrometry ◽

Liquid Chromatography Tandem Mass ◽

Commercial Milk

A liquid–liquid extraction and ultra high-performance liquid chromatography tandem mass spectrometry (UHPLC–MS/MS) method was developed for simultaneous analysis of the residues of seven neonicotinoid insecticides (NEOs), namely acetamiprid, clothianidin, dinotefuran, imidacloprid, thiacloprid, thiamethoxam, and nitenpyram, in commercial milk samples. The method had a good linearity (R2 > 0.992) and a limit of detection range of 0.004–0.15 μg/kg. The average recovery range was 89–119% with an intraday precision of 1.4–10.3% at spiking levels of 8, 12, and 16 μg/kg. The validated method was employed for routine analysis of the aforementioned seven NEOs in commercial milk samples obtained randomly from a supermarket in Miaoli (Taiwan). The detected thiamethoxam and clothianidin levels were 3.4 and 80 μg/kg, respectively.

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