Development of a Quantitative Method for Detection of Multiclass Veterinary Drugs in Feed Using Modified QuPPe Extraction and LC–MS/MS

A method was developed for the rapid and quantitative analysis of 30 veterinary drugs belonging to 17 classes (amphenicols (1), anthelmintics (1), cephalosporins (4), coccidiostats (1), lincosamides (1), macrolide (1), nitroimidazole (1), penicillins (3), phenylhydrazines (1), polypeptides (1), pyrethrins (1), quinolones (5), sulfonamides (3), tetracycline (3), neuroleptic agents (1), triazene trypanocidal agents (1), other. (1)) in feeds. The proposed method with a modified Quick Polar Pesticides (QuPPe) sample preparation was validated for the determination of 30 veterinary drugs in feed samples by liquid chromatography triple-quadrupole mass spectrometry (LC–MS/MS). The sample was extracted with methanol containing 1% acetic acid and purified by dispersive solid-phase extraction (d-SPE) with C18. Good linearity (r2 ≥ 0.98) was observed, and the LOQ values ranged from 10 to 200 µg/kg. Average recoveries ranged from 70.8 to 118.4%, and the relative standard deviation was ≤ 18.7%. This validated method was used in the determination of 30 veterinary drugs in 142 feed samples obtained from South Korea. The results show that lincomycin was present in only one of the tested feed samples, although it was detected at a value lower than the LOQ. In conclusion, this multi-residue method can be used for screening through the detection and quantitation of residual multiclass veterinary drugs in feed samples

Optimization of the QuEChERS-Based Analytical Method for Investigation of 11 Mycotoxin Residues in Feed Ingredients and Compound Feeds

Mycotoxins are toxic substances naturally produced by various fungi, and these compounds not only inflict economic damage, but also pose risks to human and animal health. The goal of the present study was to optimize the QuEChERS-based extraction and liquid chromatography–tandem mass spectrometry (LC–MS/MS) method for the analysis of 11 mycotoxins, such as aflatoxins (AFs), ochratoxin A (OTA), fumonisins (FBs), T-2 toxin, HT-2 toxin, zearalenone (ZEN), and deoxynivalenol (DON), commonly found in feed. The QuEChERS method, characterized by being “quick, easy, cheap, effective, rugged, and safe”, has become one of the most common extractions and clean-up procedures for mycotoxin analyses in food. Therefore, in this experiment, an optimal method for the analysis of 11 mycotoxins in feed was established by modifying the general QuEChERS method. In this process, it was confirmed that even if feed samples of different weights were extracted, the quantitative value of mycotoxins in the feed was not affected. To reduce matrix effects, 13C-labeled compounds and deuterium were used as internal standards. This optimized method was then applied in the determination of 11 mycotoxins in 736 feed ingredients and compound feeds obtained from South Korea. The results showed that the occurrence rates of FBs, ZEN, and DON were 59.4%, 38.0%, and 32.1%, respectively, and OTA, AFs, and T-2 toxin and HT-2 toxin were found in fewer than 1% of the 736 feeds. The mean concentration ranges of FBs, ZEN, and DON were 757–2387, 44–4552, and 248–9680 μg/kg, respectively. Among the samples in which DON and ZEN were detected, 10 and 12 samples exceeded the management recommendation standards presented by the Ministry of Agriculture, Food and Rural Affairs (MAFRA). However, when the detected concentrations of DON and ZEN were compared with guideline levels in foreign countries, such as the US, Japan, China, and the EU, the number of positive samples changed. In addition, the co-occurrence of mycotoxins in the feed was analyzed, and the results showed that 43.8% of the samples were contaminated with two or three mycotoxins, among which the co-occurrence rate of FBs, ZEN, and DON was the highest. In conclusion, these results suggest the need for stricter management standards for FBs, DON, and ZEN in South Korea, and emphasize the importance of the continuous monitoring of feeds

Optimization of the QuEChERS-Based Analytical Method for Investigation of 11 Mycotoxin Residues in Feed Ingredients and Compound Feeds

Mycotoxins are toxic substances naturally produced by various fungi, and these compounds not only inflict economic damage, but also pose risks to human and animal health. The goal of the present study was to optimize the QuEChERS-based extraction and liquid chromatography–tandem mass spectrometry (LC–MS/MS) method for the analysis of 11 mycotoxins, such as aflatoxins (AFs), ochratoxin A (OTA), fumonisins (FBs), T-2 toxin, HT-2 toxin, zearalenone (ZEN), and deoxynivalenol (DON), commonly found in feed. The QuEChERS method, characterized by being “quick, easy, cheap, effective, rugged, and safe”, has become one of the most common extractions and clean-up procedures for mycotoxin analyses in food. Therefore, in this experiment, an optimal method for the analysis of 11 mycotoxins in feed was established by modifying the general QuEChERS method. In this process, it was confirmed that even if feed samples of different weights were extracted, the quantitative value of mycotoxins in the feed was not affected. To reduce matrix effects, 13C-labeled compounds and deuterium were used as internal standards. This optimized method was then applied in the determination of 11 mycotoxins in 736 feed ingredients and compound feeds obtained from South Korea. The results showed that the occurrence rates of FBs, ZEN, and DON were 59.4%, 38.0%, and 32.1%, respectively, and OTA, AFs, and T-2 toxin and HT-2 toxin were found in fewer than 1% of the 736 feeds. The mean concentration ranges of FBs, ZEN, and DON were 757–2387, 44–4552, and 248–9680 μg/kg, respectively. Among the samples in which DON and ZEN were detected, 10 and 12 samples exceeded the management recommendation standards presented by the Ministry of Agriculture, Food and Rural Affairs (MAFRA). However, when the detected concentrations of DON and ZEN were compared with guideline levels in foreign countries, such as the US, Japan, China, and the EU, the number of positive samples changed. In addition, the co-occurrence of mycotoxins in the feed was analyzed, and the results showed that 43.8% of the samples were contaminated with two or three mycotoxins, among which the co-occurrence rate of FBs, ZEN, and DON was the highest. In conclusion, these results suggest the need for stricter management standards for FBs, DON, and ZEN in South Korea, and emphasize the importance of the continuous monitoring of feeds

Elucidating the Chain-Extension Effect on the Exciton-Dissociation Mechanism through an Intra- or Interchain Polaron-Pair State in Push???Pull Conjugated Polymers

We elucidated chain-extension effects of a benzodithiophene (BDT) and thienopyrroledione-based push???pull conjugated polymer (CP) on its exciton-dissociation mechanism within aggregate systems using transient absoption spectroscopy. The side-group extension CP with benzothiophene on the BDT unit induced H-type excitons with excess energy owing to decreased chain stiffness. This led to interchain polaron-pair (PP)-mediated exciton dissociation. The stiff side-group extended with thienothiophene on the BDT unit also induced H-type excitons, but the decreased energy and breadth of the density of states suppressed the interchain PP-mediated exciton dissociation. The main-chain-extension CP with two thiophenes on either side of the BDT unit has a curved structure disturbing the interchain packing. Thus, the driving force of exciton dissociation between the chains decreased, leading to intrachain PP-mediated exciton dissociation. Our findings can facilitate the development of novel CPs to further increase the efficiencies of polymer solar cells

Elucidating the Chain-Extension Effect on the Exciton-Dissociation Mechanism through an Intra- or Interchain Polaron-Pair State in Push–Pull Conjugated Polymers

We elucidated chain-extension effects of a benzo-dithiophene (BDT) and thienopyrroledione-based push-pull conjugated polymer (CP) on its exciton-dissociation mechanism within aggregate systems using transient absoption spectroscopy. The side-group extension CP with benzothiophene on the BDT unit induced H-type excitons with excess energy owing to decreased chain stiffness. This led to interchain polaron-pair (PP)-mediated exciton dissociation. The stiff side-group extended with thienothiophene on the BDT unit also induced H-type excitons, but the decreased energy and breadth of the density of states suppressed the interchain PP-mediated exciton dissociation. The main-chain-extension CP with two thiophenes on either side of the BDT unit has a curved structure disturbing the interchain packing. Thus, the driving force of exciton dissociation between the chains decreased, leading to intrachain PP-mediated exciton dissociation. Our findings can facilitate the development of novel CPs to further increase the efficiencies of polymer solar cells.11Nsciescopu

Elucidating the Chain-Extension Effect on the Exciton-Dissociation Mechanism through an Intra- or Interchain Polaron-Pair State in Push–Pull Conjugated Polymers

We elucidated chain-extension effects of a benzodithiophene (BDT) and thienopyrroledione-based push–pull conjugated polymer (CP) on its exciton-dissociation mechanism within aggregate systems using transient absoption spectroscopy. The side-group extension CP with benzothiophene on the BDT unit induced H-type excitons with excess energy owing to decreased chain stiffness. This led to interchain polaron-pair (PP)-mediated exciton dissociation. The stiff side-group extended with thienothiophene on the BDT unit also induced H-type excitons, but the decreased energy and breadth of the density of states suppressed the interchain PP-mediated exciton dissociation. The main-chain-extension CP with two thiophenes on either side of the BDT unit has a curved structure disturbing the interchain packing. Thus, the driving force of exciton dissociation between the chains decreased, leading to intrachain PP-mediated exciton dissociation. Our findings can facilitate the development of novel CPs to further increase the efficiencies of polymer solar cells