Targeted analysis and determination of β‐agonists,hormones, glucocorticoid and psychiatric drugs in feed by liquid chromatography with electrospray ionization tandem mass spectrometry

A comprehensive strategy combining a quantitative method was developed for 30 banned drugs including β‐agonists, hormones, glucocorticoid and psychiatric drugs in swine and chicken feeds. This rapid, simple and effective extraction method was based on matrix solid‐phase dispersion and electrospray ionization tandem mass spectrometry. The quantitative method was validated after previous statistical optimization of the main parameters of matrix solid‐phase dispersion. The limit of quantification of dopamine hydrochloride, chlormadinone acetate, melengestrol acetate, testosterone propionate, nandrolone and midazolam was 2 μg/kg and that of the other 24 drugs was 1 μg/kg. The recoveries of β‐agonists, hormones, glucocorticoid and psychiatric drugs spiked in swine and chicken feeds at a concentration range of 1–8 μg/kg were above 70.1% with inter‐day relative standard deviations less than 15.8%. The analytical strategy was applied to 100 feed samples collected from a local market in Wuhan (China). Clenbuterol, ractopamine and melengestrol acetate were identified and quantified at the level 0.2～3.5 μg/kg. The rapid and reliable method can be used to efficiently separate, characterize and quantify the residues of 30 banned drugs in swine and chicken feeds with advantages of simple pretreatment and environmental friendly nature.     

高效液相色谱-串联质谱法同时测定饲料中9种霉菌毒素及其代谢物

应用高效液相色谱-串联质谱(HPLC-MS/MS)技术,建立了同时检测饲料中9种霉菌毒素及其代谢物的分析方法。样品加入NaCl经乙腈-水(85∶15)振荡提取后,用TC-M160多功能净化柱净化,氮气吹干,用1mL乙腈-水(1∶1)定容,Agilen C18色谱柱(150×2.1mm,3.5μm)分离,采用正负离子同时扫描的多反应监测模式进行检测,外标法定量。方法检出限为0.11~0.60μg/L,在2.0~100.0μg/L基质添加浓度范围内呈现良好的线性关系,相关系数r0.998。5.0~50.0μg/L加标范围内回收率为67.0%~103.5%,相对标准偏差15%。该法简便、快速、灵敏度高,符合对饲料中霉菌毒素的检测要求,可为相关检测提供技术支持。     

船载C+S频段共面单脉冲天线设计与应用

本文针对船载测控站空间狭小的特点,介绍了一种C+S双频段共面天线的设计。设计时采用了计算机辅助技术,确定了天线反射面和馈源喇叭的形式及相对关系尺寸。并通过仿真计算和实测结果,该天线在两个频段的方向图指标均满足设计要求,达到了天线的小型化和双频段合建目的,满足航天测量船船载设备的使用要求。     

Hydrogels with Dynamically Controllable Mechanics and Biochemistry for 3D Cell Culture Platforms

Many cell-matrix interaction studies have proved that dynamic changes in the extracellular matrix(ECM)are crucial to maintain cellular properties and behaviors.Thus,developing materials that can recapitulate the dynamic attributes of the ECM is highly desired for threedimensional(3 D)cell culture platforms.To this end,we sought to develop a hydrogel system that would enable dynamic and reversible turning of its mechanical and biochemical properties,thus facilitating the control of cell culture to imitate the natural ECM.Herein,a hydrogel with dynamic mechanics and a biochemistry based on an addition-fragmentation chain transfer(AFCT)reaction was constructed.Thiol-modified hyaluronic acid(HA)and allyl sulfide-modifiedε-poly-L-lysine(EPL)were synthesized to form hydrogels,which were non-swellable and biocompatible.The reversible modulus of the hydrogel was first achieved through the AFCT reaction;the modulus can also be regulated stepwise by changing the dose of UVA irradiation.Dynamic patterning of fluorescent markers in the hydrogel was also realized.Therefore,this dynamically controllable hydrogel has great potential as a 3 D cell culture platform for tissue engineering applications.     

Determination of 1-Lysine in Feeds by Fluorometric Method Based on 1-Lysine Oxidase

Abstract

Feeds or feed stuffs were hydrolyzed by acid to liberate 1-lysine. Homovanillic acid, peroxidase and 1-lysine oxidase were used to produce the fluorescence substance corresponding to 1-lysine. A computerized fluorometer was used for the measurement (up to 0.7 mg/1 of 1-lysine in the optical cell) and the time required for the measurement was about 1 min. The reproducibility was 1.0% in CV. Recovery tests and comparative tests against the conventional method were carried out. The effects of various experimental conditions on the fluorescence response were discussed.     

Radio-Detoxication of Olive Cake

The possibility of reducing toxic substances in olive by-products subjected as animal feed stuffs after oil extraction was investigated.

Total phenols in fresh olive fruits were 0.6%(fruit),0.7%(woody pit) and 0.31%in cakes after extraction. Irradiation of the olive cake powder at different doses (0,10,50 and 100 kGy) was done as a trial to remove the toxic substances. The results proved that irradiation decreases total phenols of olive cake from 0.31% (control) to 0.21, 0.16 and 0.08%at the doses used, respectively.

Subcutaneously injected ethanolic extract of unirradiated or irradiated (with 10 kGy) olive cake was lethal to the rats, while at 50 and 100 kGy all rats survived.

Liver and heart functions were measured in terms of activities of glutamate oxaloacetate transaminase (GOT), glutamate pyruvate transaminase (GPT), total protein and lactic acid dehydrogenase (LDH). In addition, plasma total lipids, cholesterol, triglycerides, glucose and blood heamoglobin were measured.

Results obtained showed that the toxic substances in olive cake induced toxicosis symptoms with the experimental rats treated with the irradiated (50 kGy) samples. The toxic compounds could be destroyed at an irradiation dose level of 100 kGy without harmful effects on liver and heart functions as well as heamoglobin, carbohydrate and lipid metabolisms. After further investigations, irradiation with 100 kGy shall be recommended to be used for detoxication of olive by-products for animal feeding without deleterious side effects.     

Multiclass,multiresidue method for the detection of antibiotic residues in distillers grains by liquid chromatography and ion trap tandem mass spectrometry

The increased production of ethanol in the US has resulted in large amounts of distillers grains (DG) which is an excellent feed supplement for livestock. However, the use of antimicrobials during ethanol fermentation has led to a growing concern over the possibility of their residues remaining in DG. To enable the detection of antimicrobial residues, a robust LC–MS/MS method was developed that included 13 antibiotics of diverse chemistries, ampicillin, penicillin G, tetracycline, oxytetracycline, chlortetracycline, bacitracin A, virginiamycin M1, chloramphenicol, erythromycin A, clarithromycin, tylosin A, monensin A and streptomycin. The residues were extracted with an aqueous solution of EDTA and trichloroacetic acid followed by methanol. The combined extract was subjected to a two-track cleanup and concentration on either hydrophilic polymeric or weak cation exchange solid phase extraction cartridges. The extracts are analyzed by LC/ion trap tandem mass spectrometry. The method was validated in dry DG matrix. Absolute recoveries of the analytes ranged from 50 to 100%. Accuracy ranged from 89 to 111% based on calibration by processed standards. The limits of detection and relative standard deviation are satisfactory to support future surveillance studies. The method was subsequently tested in three different end-products of DG: distillers dry grains, distillers wet grains and distillers grains solubles.     

军用化工企业含氮废水处理工艺研究

采用厌氧——缺氧——SBR微生物生化处理组合工艺,研究了双基（含双基混合酯）球扁药含氮废水处理技术,通过菌种驯化,实现了高盐浓度、高CODCr含量废水经处理后达标排放,CODCr的总去除率达到97．7％,质量浓度降到96mg／L;BOD5总去除率达到了98．O％,质量浓度降到28mg／L;SS的总去除率达到94．4％,质量浓度降到了9mg／L。     

UPLC-MRM法测定饲料中的三聚氰胺

提出了一种UPLC-MRM测定饲料中微量三聚氰胺的分析方法. 饲料经10 g/L三氯乙酸溶液提取和22 g/L乙酸铅溶液沉淀蛋白质, 过混合型阳离子交换柱(MCX)纯化, 离心后用0.45 μm滤膜过滤, 用超高效液相色谱-质谱-质谱联用仪(UPLC-MS-MS)分析测定, 以三聚氰胺母离子126.9 (m/z)和子离子67.5与84.6 (m/z)定性、定量目标物. 饲料样品加标回收率(n=6)为84.5%, 检测限0.01 μg/L, 相对偏差(RSD) 6.5%.     

Development of a matrix solid-phase dispersion method for the simultaneous determination of pyrethroid and organochlorinated pesticides in cattle feed

A matrix solid-phase dispersion (MSPD) method was developed for the simultaneous extraction of 36 common pesticides and breakdown products (mostly pyrethroids and organochlorines) in cattle feed. Different parameters affecting the extraction efficiency (such as dispersing phase, clean-up adsorbent and elution volume) were investigated. The experimental procedure was optimized using a multivariate statistical approach and the final analyses were carried out by GC-muECD. Several protocols for extract purification were also studied. As far as we know, this is the first application of MSPD for the extraction of most of the target pesticides from animal feed. Using the optimized extraction conditions, the method was validated in terms of accuracy, and precision (within-a-day and among-days), using a certified reference material (CRM 115) as well as spiked cattle feedingstuffs at different concentration levels. A matrix effect study was also carried out using various real samples. The recoveries were satisfactory (>75% in most cases) and the quantification limits, at the sub-ngg(-1) or low-ngg(-1) level, complied with the regulated maximum residue levels (MRLs) in animal feed and in main crops used in the preparation of cattle feeding materials. Finally, the MSPD-GC-muECD methodology was applied to the analysis of real cattle feed samples collected in farms of dairy cattle from NW Spain.