分散固相萃取-超高效液相色谱-串联质谱联用快速检测玉米及土壤中莠去津残留

采用分散固相萃取（QuEChERS）为样品前处理方法,建立了超高效液相色谱-串联四极杆质谱快速检测玉米及土壤中莠去津残留分析方法。玉米及土壤样品经乙腈提取、乙二胺-N-丙基硅烷（PSA）分散固相（DSPE）净化后,应用超高效液相色谱/电喷雾串联四极杆质谱仪多离子反应监测（MRM）定量检测,分别以碎片离子m/z216〉146和m/z216〉174定性,以m/z216〉96进行外标法定量。结果表明,在0.005～0.5mg·kg^-1添加水平范围内莠去津的平均添加回收率在77.01%～112.62%之间,相对标准偏差在2.23%～8.43%之间,对莠去津的检出限（LOD）为0.39～0.91μg·kg^-1,定量检出限（LOQ）为1.33～3.02μg·kg^-1。该方法灵敏度高,操作简单,定量准确,测定浓度范围宽,可用于莠去津的残留分析。     

甲砜霉素在鲤鱼及鲫鱼体内的残留研究

本研究旨在分析甲砜霉素在鲤鱼和鲫鱼体内的残留消除规律并为制定休药期提供依据。按照30 mg/kg的给药量对鲤鱼和鲫鱼连续口灌给药甲砜霉素3天,定时取样,外标法定量,采用高效液相色谱-串联质谱法(HPLC-MS/MS)检测采样组织中甲砜霉素的残留量。结果显示：甲砜霉素在0.1~200 ng/mL范围内有良好的线性关系,相关系数为0.9987。回收率在81.33%~109.72%之间。甲砜霉素在停止给药后鱼体各检测组织中残留量呈下降趋势,在停药25天后,甲砜霉素残留量低于中国与欧盟规定的最高残留限量(MRLs)。根据结果,建议休药期为25天。     

UASB工艺处理高浓度Vc生产废水的试验研究

采用UASB反应器对高浓度Vc生产废水进行了实验室处理研究。试验结果表明:Vc废水的厌氧处理运行性能因水质不同而存在很大差异。转化母液的容积负荷在8kg COD.m-3d-1以下时,去除率基本稳定在65%以上。当负荷继续提高时,去除率会急剧下降并保持在50%左右。精制母液和提取母液的容积负荷在10kgCOD.m-3d-1时去除率仍能稳定在70%以上。这些表明当两套反应系统的容积负荷控制在一定范围时,UASB反应器可以有效去除大部分的有机污染物。同时也说明转化母液废水中存在相当数量的难生物降解化合物。GC/MS水质分析结果表明,其中含有大量10C以上的长直链或双苯环等结构的难生物降解物。系统中厌氧颗粒污泥的产甲烷活性随着反应器中污泥驯化的进行和负荷的增加而上升。     

40%乙酰甲胺磷乳油在青油菜和土壤中的消解动态研究

为了评价乙酰甲胺磷在蔬菜上使用后的环境行为和环境安全性,采用GC/MS测定方法,研究了40%乙酰甲胺磷乳油在青油菜和土壤环境中的消解动态规律和最终残留。结果表明：乙酰甲胺磷在降解过程中可转化为甲胺磷,乙酰甲胺磷和甲胺磷在青油菜上的降解半衰期分别为1.36d、2.86d,在土壤中的降解半衰期分别为1.84d、2.96d,乙酰甲胺磷降解速率比甲胺磷快,在正常使用条件下,不会造成环境的累积和污染     

小麦籽粒B族维生素含量及其与籽粒色素的相关分析研究

小麦籽粒含有多种B族维生素,本研究通过测定24个不同粒色的小麦品种中维生素B1、维生素B2、维生素B6及籽粒色素含量,并研究不同颜色的小麦籽粒中B族维生素含量与小麦籽粒颜色的关系及其变异规律,为B族维生素的利用及小麦品质育种提供依据。应用超高效液相色谱-串联质谱法,采用大气压电喷雾离子源,正离子模式,多反应检测（MRM）模式精确测定小麦籽粒中维生素B1、维生素B2、维生素B6,分光光度法测定小麦籽粒色素含量。黑小麦76和VICTO杂交后代F8代12个姊妹系B族维生素含量变化很大,12个姊妹系间维生素B1、维生素B2、维生素B6的含量差异达极显著水平。冬鉴系列的10个小麦品种（系）维生素B1、维生素B2、维生素B6的含量差异达显著水平。相关分析表明,籽粒色素含量与B族维生素含量不存在显著正相关,籽粒颜色深小麦并不一定富含B族维生素。小麦籽粒中B族维生素含量受基因型的影响, 可以通过遗传改良的手段提高B族维生素在小麦籽粒中的含量。黑小麦76（母本）和VICTO（父本）杂交产生的F8代12个姊妹系的小麦籽粒中B族维生素含量存在着明显的超高亲杂种优势,因此,可通过有性杂交,培育高B族维生素含量的小麦品种。     

Regeneration of adventitious shoots from mature stored cotyledons of Japanese plum (Prunus salicina Lind1)

Adventitious shoot regeneration from mature stored cotyledons of Japanese plum (Prunus salicina Lind1) was achieved in vitro. The influences of the presence and absence of the light, different concentrations of thidiazuron (TDZ) and benzyladenine (BA) in the culture media, TDZ pretreatments and different basal salts on shoot regeneration were evaluated. TDZ was more effective in inducing shoot regeneration from mature stored cotyledons than BA. Dark incubation significantly increased the regeneration frequencies. Quoirin/Lepoivre (QL) basal salts stimulated shoot regeneration more than woody plant (WPM) or B5 salts did. The frequency of adventitious shoot formation varied among the varieties and the regeneration ability appeared to be genotype depended. The frequency of regeneration under the optimum tested conditions for ‘Bruce’, ‘Shiro’, ‘Redheart’, ‘Gladstone’ and ‘Early Golden’ cotyledons were 66.7%, 46.7%, 43.3%, 26.7% and 6.7%, respectively.     

Disulphide structure of high-molecular-weight (HMW-) gliadins as affected by terminators

This study aimed at elucidating SS-bonds of HMW-gliadins (HGL) from wheat with the focus on terminators of glutenin polymerisation. HGL from wheat flour extracts non-treated or treated with the S-alkylation reagent N-ethylmaleinimide (NEMI) were compared. HGL from wheat flour Akteur were isolated, hydrolysed with thermolysin and the resulting peptides pre-separated by gel permeation chromatography and analysed by liquid chromatography/mass-spectrometry using alternating electron transfer dissociation/collision-induced dissociation. Altogether, 22 and 28 SS-peptides from samples without and with NEMI treatment, respectively, were identified. Twenty-six peptides included standard SS-bonds of α- and γ-gliadins, high-molecular-weight and low-molecular-weight glutenin subunits. Eleven SS-bonds were identified for the first time. Fifteen peptides unique to HGL contained cysteine residues from gliadins with an odd number of cysteines (ω5-, α- and γ-gliadins). Thus, gliadins with an odd number of cysteines, glutathione and cysteine had acted as terminators of glutenin polymerisation. Decisive differences between samples without and with NEMI treatment were not obvious showing that the termination of polymerisation was already completed in the flour. The two HGL samples, however, were different in the majority of ten peptides that included disulphide-linked low-molecular-weight (LMW) thiols such as glutathione and cysteine with the former being enriched in the non-treated HGL-sample.     

5种动物源食品中的氟虫腈及其3个代谢物残留量检测

利用QuEChERS技术结合超高效液相色谱-串联质谱的方法检测5种动物源食品(鸡肉、鸡蛋、猪肝、牛奶、猪肉)中氟虫腈及其3个代谢物残留量。样品用乙腈提取,经低温处理,多壁碳纳米管(MWCNTs)、弗罗里硅土(Florisil)和C18分散固相萃取(d-SPE)净化,外标法定量。在不同浓度的加标水平下,氟虫腈及其代谢物在5种动物源食品中的平均回收率为72.1%～113.8%,相对标准偏差RSD为1.9%～17.6%,检出限LOD在0.73～1.94μg/kg范围内,定量限LOQ在5～10μg/kg范围内。该方法具有简单、灵敏、准确等优点,适用于动物源食品中氟虫腈及其代谢物的快速筛查和定量检测。     

Soil volatile fungistasis and volatile fungistatic compounds

Fungistasis is a widespread phenomenon that can be mediated by soil microorganisms and volatile organic compounds (VOCs). The relationship between soil microorganisms and VOCs is still unclear, however, and many fungistatic compounds remain to be identified. We assessed the effects of soils (soil direct fungistasis) and VOCs produced by natural soils (soil volatile fungistasis) on the spore germination of several fungi. Both strong soil direct fungistasis and soil volatile fungistasis were observed in a wide range of soils. Soil fungistasis and VOC fungistasis were significantly correlated (P<0.001). The volatile fungistatic activity of soils stopped after autoclaving. Some VOCs were identified by using solid-phase microextraction-gas chromatography/mass spectrum. VOC composition and in vitro antagonism of relatively pure commercial compounds also were measured. Some VOCs, trimethylamine, 3-methyl-2-pentanone, dimethyl disulfide, methyl pyrazine, 2,5-dimethyl-pyrazine, benzaldehyde, N,N-dimethyloctylamine and nonadecane, were produced by various fungistatic soils. Moreover, antifungal activity test of above VOCs showed that trimethylamine, benzaldehyde, and N,N-dimethyloctylamine have strong antifungal activity even at low levels (4-12 mg l⁻¹).     

Theonellamides J and K and 5-cis-Apoa-theopalauamide,Bicyclic Glycopeptides of the Red Sea Sponge Theonella swinhoei

Theonella swinhoei is a fairly common inhabitant of reefs throughout the Indian and Pacific Oceans. Metabolomic analyses of samples of T. swinhoei collected in different depths in the Gulf of Aqaba revealed two chemotypes differing in the profiles of the theonellamides they produce, some of which seem to be unknown. Driven by this finding, we examined a sample of T. swinhoei collected more than 40 years ago in the southern part of the Gulf of Aqaba. Large-scale extract of this sample yielded four theonellamides, the known theopalauamide (4), as the major component, and three new metabolites, theonellamide J (1), 5-cis-Apoa-theopalauamide (2), and theonellamide K (3), as the minor components. The planar structure of these complex cyclic glycopeptides was elucidated by combination of 1D and 2D NMR techniques and HRESIMS. The absolute configuration of the amino acids was established by Marfey’s and advanced Marfey’s methods, and the absolute configuration of its galactose unit using “Tanaka’s method” for monosaccharides. The biological activity of the pure compounds was tested for antibacterial activity and for cytotoxicity to HTC-116 cell line. The compounds presented significant cytotoxicity against the HTC-116 cell line, illuminating the importance of the Apoa subunit for the activity.