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.     

流图的反馈回路结构分析方法

运用系统动力学研究复杂系统,通常必须了解该系统的流图的反馈回路的结构,而目前计算反馈回路的方法比较复杂,通过将强简化流率基本入树的每棵树转换成树向量,树向量构成矩阵,并定义矩阵相关元素的运算,可比较简单地算出流图的各阶反馈回路的条数,从而揭示流图的反馈回路结构的性质.     

Hydrogen production capacity of membrane reformer for methane steam reforming near practical working conditions

Currently, H₂ production techniques for application to proton exchange membrane fuel cells (PEMFC) are intensively investigated, aiming to realize a clean hydrogen society. Due to the limitation by the thermodynamics of methane steam reforming (MSR), multi-reactions and multi-steps should be performed before the generated H₂-rich gas could be delivered to PEMFC, which inevitably increases the cost of H₂. However, using a thermodynamic shifting membrane reformer, H₂ could be produced compactly from MSR, provided that the catalyst showed high performance for MSR reaction and membrane efficiently removed H₂ from the reaction zone. We presented here a Pd-based membrane reformer for MSR reaction. In contrast with previous reports, nickel-based catalyst pre-reduced at high temperature was applied in this work, as well as high performance Pd-based membrane. The performances of the membrane reformer in terms of H₂ production capacity were also widely investigated. It was found that combination of an active catalyst for MSR and a H₂ ultra-permeable Pd membrane obtained high flux of H₂ across the membrane and recovery rate of H₂ in the membrane reformer. For instance, 98.8% methane conversion, over 97.0% selectivity to CO₂ and over 95.0% recovery rate of H₂ were obtained under mild working conditions. Simultaneously, the hydrogen flux across the membrane reached 18.6 m³/(m² h), and Pd-based pure H₂ production capacity significantly increased and reached around 387.5 m³/(kg_Pd h) in membrane reformer. Further work on stability investigation may develop an efficient on-site route of H₂ production process for application to on-site power generation using PEMFC.     

二维磁流体力学程序MFCGⅢ计算结果与测试结果的对比分析

 根据磁场、流函数和感应电流的解析公式，研制了间接馈电爆磁压缩发生器充电和爆磁压缩过程计算程序MFCGⅢ。用MFCGⅢ计算了实验模型，其结果与测试结果符合较好。因此MFCGⅢ可对实验提供优化设计，并且可分析、解释MFCG实验中有关的物理问题。     

Determination of synephrine in feeds by a novel quick,easy, cheap,effective, rugged,and safe solid‐phase extraction method combined with UHPLC–MS/MS

To detect and quantify synephrine in feed, an effective analytical method based on quick, easy, cheap, effective, rugged, and safe solid‐phase extraction coupled to ultra high performance liquid chromatography with tandem mass spectrometry was developed with isotopic internal standards. Pretreatment was performed using quick, easy, cheap, effective, rugged, and safe solid‐phase extraction with primary secondary amine and C18 sorbent as sorbents in combination with Oasis MCX column clean‐up to extract and purify feed samples. Tandem mass spectrometry detection in positive ion mode was conducted in positive multiple reaction monitoring mode in addition to the quantitative internal standard method. Two transitions of synephrine at m/z 168.1/150.0 and 168.1/135.0 were selected, and m/z 168.1/135.0 was determined as the quantification ion pair. D₉‐Terbutaline was selected as an internal standard, for which m/z 235.1/153.0 was selected as the quantification ion pair. Good linearity was shown for synephrine in the range of 0.5–50 μg/L, and the correlation coefficient exceeded 0.999. The recoveries in three different feed samples at three spiked levels were 81.42–112.08%, and the relative standard deviations were not greater than 14.66%. The method proposed in this study was reliable and highly effective, and its sensitivity, accuracy, and precision are suitable for determining synephrine residues in feed samples.     

Comparison of different extraction techniques for the determination of chlorinated pesticides in animal feed

The performances of Soxhlet extraction, dive-in Soxhlet extraction, microwave-assisted extraction (MAE), accelerated solvent extraction (ASE), fluidized-bed extraction (FBE), and ultrasonic extraction (UE) for the analysis of organochlorine pesticides in animal feed have been investigated. ASE and MAE provided significantly better extraction efficiency than Soxhlet extraction. The concentrations were 126.7 and 114.8%, respectively, of the values obtained by classical Soxhlet extraction, whereas the results from FBE and dive-in Soxhlet were comparable with those from the standard Soxhlet procedure. The reproducibility of FBE was the best, with RSDs ranging from 0.3 to 3.9%. Under the investigated operation conditions UE was not efficient, with the recoveries of target compounds being about 50% less than Soxhlet. Additionally, the performances of Soxhlet, dive-in Soxhlet, MAE, ASE and FBE were validated by determination of the certified reference material BCR-115. The results from the extraction techniques were in good agreement with the certified values.     

Comparison of extraction techniques of robenidine from poultry feed samples

In this paper, effectiveness of six different commonly applied extraction techniques for the determination of robenidine in poultry feed has been compared. The sample preparation techniques included shaking, Soxhlet, Soxtec, ultrasonically assisted extraction, microwave – assisted extraction and accelerated solvent extraction. Comparison of these techniques was done with respect to the recovery extraction, temperature and time, reproducibility and solvent consumption. Every single extract was subjected to clean – up using aluminium oxide column (Pasteur pipette filled with 1 g of aluminium oxide), from which robenidine was eluted with 10 ml of methanol. The eluate from the clean-up column was collected in a volumetric flask, and finally it was analysed by HPLC–DAD–MS. In general, all extraction techniques were capable of isolating of robenidine from poultry feed, but the recovery obtained using modern extraction techniques was higher than that obtained using conventional techniques.

In particular, accelerated solvent extraction was more superior to other techniques, which highlights the advantages of this sample preparation technique. However, in routine analysis, shaking and ultrasonically assisted extraction is still the preferred method for the solution of robenidine and other coccidiostatics.     

反相高效液相色谱法测定饲料中尼卡巴嗪含量

用二甲基甲酰胺(DMF)提取试样中的尼卡巴嗪，经碱性氧化铝层析柱过柱纯化、浓缩，并用洗脱液溶解、定容，用高效液相色谱仪C18反相柱，在波长365nm、流速1mL/min条件下对饲料中尼卡巴嗪含量进行测定。通过对氧化铝活性、层析柱高度、流动相等检测条件对比试验，建立的理想检测条件为：105℃恒温干燥2h处理高度6cm的氧化铝柱，采用的流动相甲醇：水为80：20。应用建立的测试方法，对饲料添加100mg／kg尼卡巴嗪进行30次重复试验。结果表明，尼卡巴嗪回收率在91．9％～107．5％之间，标准偏差4．0％。研究还表明，饲料中其它常用的抗球虫药盐霉素、马杜霉素、地克珠利对该检测无任何干扰。     

熔融碳酸盐燃料电池系统中重整器性能分析

本文通过对热交换型重整器过程分析，建立了反映其性能的动态数学模型，并进行了稳态与动态模拟计算．结果表明，重整产物气能满足熔融碳酸盐燃料电池需要，同时也得到了水蒸气与天然气之比对重整产物成分的影响；研究了过程气入口流量、温度改变时重整器动态响应性能，为控制回路的制定提供了理论依据．     

The application of multielemental analysis in the elaboration of technology of mineral feed additives based on Lemna minor biomass

Supplementation of microelements (Mn, Zn, Cu, Cr) to livestock diet is of particular concern. There are various mineral feed additives available on the market. The most frequently used are inorganic feed additives, characterized with low bioavailability and high toxicity. Also, organic feed additives are used, including amino acids chelates, in which bioavailability was greatly improved and toxicity reduced. The problem is high price of these products. Therefore, there is the need to search for new biological mineral feed additives with designed composition, that would be characterized with high bioavailability, low toxicity, low cost and that would also possess a nutritional value. Such a possibility offers biological materials. It was found that biomaterials have metal-binding capabilities. Metal ions may be bound to biomass via either biosorption or bioaccumulation process.

When elaborating technology of the production of feed additives, containing simultaneously various elements, it is necessary to use the tool of multielemental analysis in order to simultaneously analyze the content of Mn, Zn, Cu, Cr. In the present work, ICP-OES multielemental analysis was used to investigate the process of production of mineral feed additives based on the biomass of aquatic plant Lemna minor. The effectiveness of the processes of biosorption and bioaccumulation of microelements by an aquatic plant L. minor was studied. The mechanism of the process as well as equilibrium was investigated with the use of multielemental analysis by ICP-OES Vista-MPX instrument from Varian (Australia).