农药残留检测中不同蔬菜的基质效应

基于QuEChERS前处理方法,在气相色谱-串联质谱 (GC-MS/MS) 和超高效液相色谱-串联质谱 (UPLC-MS/MS) 检测条件下,考察了200种农药在17种蔬菜基质中的基质效应,通过基质效应分析找到了合适的代表性基质用作配制检测过程中的基质匹配标准溶液。结果表明:由于基质干扰成分及农药性质的差异,导致不同蔬菜及农药品种之间的基质效应差异。在GC-MS/MS检测中,供试的150种农药中绝大部分表现为基质增强效应,其中葱、姜和大蒜表现为很强的基质效应,萝卜的基质效应较弱;菠菜、芹菜、豇豆和生菜4种蔬菜对其他蔬菜品种能够起到很好的基质校正效果,可作为代表性基质在日常检测中用于其他蔬菜基质的定量分析。在UPLC-MS/MS检测中,供试的105种农药中大部分表现为基质抑制效应,其中姜、大蒜、葱、芹菜、韭菜和菠菜的基质效应较强,西葫芦的基质效应弱;黄瓜、普通白菜、番茄和生菜4种蔬菜能较好地校正其他蔬菜的基质效应,但与GC-MS/MS相比校正能力稍弱。本研究结果认为代表性蔬菜基质可用于降低基质效应对检测结果的干扰。     

土质、温度和土壤湿度对丁草胺消散的影响

丁草胺(N-丁氧甲基-α-氯-2,6-二乙基乙酰替苯胺)用于直播水稻田和旱稻田,测定它在两种土壤(壤土和粉砂粘壤土)中的消散,测定土壤湿度和温度对丁草胺消散的影响,也进行了实验室研究。实验室和田间研究都表明,丁草胺在两种土壤中呈指数性质消散,并非常迅速。处理后21天只能测到大约1ppm,处理后70天基本上没有除草剂存在。通常,土壤湿度和温度越高,丁草胺的消散越快。     

超高效液相色谱-串联质谱法测定9种绿叶类蔬菜中36种农药多残留的基质效应

应用超高效液相色谱-串联质谱法 (UPLC-MS/MS) 研究了香菜、木耳菜、油麦菜、冬苋菜、蕹菜、生菜、芹菜、菠菜和茼蒿等9种绿叶菜类蔬菜中36种农药多残留的基质效应及影响因素。比较了QuEChERS方法中不同吸附剂对基质效应的影响,并比较了经QuEChERS方法、氨基柱净化法和未经净化直接检测3种前处理方法在UPLC-MS/MS检测模式下基质效应的差异。结果表明:N-丙基乙二胺 (PSA) 对绿叶菜中主要影响基质效应的杂质净化效果较好;QuEChERS净化法优于其他2种,样品经QuEChERS法净化后,36种农药在木耳菜、油麦菜、冬苋菜、蕹菜和生菜中均为弱基质效应,可直接采用试剂标准品进行定量分析。对于基质效应明显的蔬菜和农药,建议采用基质匹配标准曲线进行定量分析;针对一些基质效应较强的农药,在灵敏度和仪器检出限允许的前提下,可适当采用稀释法补偿基质效应。     

四种除草剂在水稻上的消解及残留规律研究

为研究四种水稻用除草剂(苄嘧磺隆、吡嘧磺隆、丙草胺、丁草胺)的消解及残留规律,建立了四种除草剂在土壤、糙米、稻壳中的分析检测方法:四种除草剂在各基质中三个添加水平的回收率均在70%-110%范围内,变异系数在1.5%-14.9%之间;基质标准曲线在0.01~1mg/kg的线性范围内,可决系数均在0.98以上,线性相关性良好,可满足检测要求。土壤检测结果显示按照推荐剂量和二倍推荐剂量施药10d后,四种除草剂的残留量均小于本方法定量限;四种除草剂最终残留量均小于糙米中最低残留限量,表明在水稻上按照推荐剂量使用这四种除草剂是安全的。     

丁西颗粒剂及其施用技术

水稻本田常用的除草剂较多,我省已应用的有恶草灵、杀草丹 2甲4氯、杀草丹、丁草胺等。其中恶草灵药源较紧,杀草丹 2甲4氯农户要买两种除草剂方能使用,杀草丹或丁草胺对阔叶杂草防效较差。5.3％丁西颗粒剂为4％丁草胺 1.3％西草净混合颗粒剂,系东清乐吉化工厂生产,具有药源立足省内,杀草谱较广,使用方便等优点,经试验示范后为农户所欢迎。现据试验示范和2.4万亩推广结果,总结如下。 (一)对水生动物的毒性     

蔬菜中13种有机磷农药基质效应研究

有机磷农药在农业生产中广泛应用,用气相色谱法进行农药残留检测容易产生基质效应,影响分析结果的可靠性,为研究用气相色谱法进行农残检测过程中有机磷农药在不同蔬菜中的基质效应,选取瓜类、茄果类、叶菜类3类常见蔬菜和13种有机磷农药进行研究,对影响基质效应的因素采取不同变量法进行分析,得出结论:有机磷农药在叶菜类蔬菜中基质效应最大;含有P=O键农药基质效应更强;基质含量越多基质效应越强,并对在检测如何减少基质效应给出了建议.     

稻田恶性杂草主要生物学特性和大面积化学防除的研究

我省处于亚热带与暖温带的过渡地带,耕作制度复杂多变,生产水平和社会经济水平差异大。按照农业生态的不同划分为太湖、沿江、沿海、里下河、徐淮等五大稻区。江苏的自然条件有利于各种杂草的发生,且危害严重。从六十年代开始先后引进了除草醚、2.4-D丁酯、敌稗、2甲4氯、杀革丹、扑草净、敌草隆、禾大壮、丁草胺、莎扑隆等除草剂进行试验,并首先在一些国营农场,如练湖、黄海等农场及部分公社,如东海县的黄川     

稻田除草剂水体残留对水生植物大薸的影响

采用模拟方法研究了稻田3种常用除草剂丁草胺、苄嘧磺隆、2甲4氯钠残留水体对大薸生长的影响。结果显示:(1)3种除草剂水体残留对大薸植株形态影响以苄嘧磺隆处理最为明显,残留浓度大于0.01 mg/L可导致大薸植株大量死亡。4.25 mg/L的丁草胺和3.36 mg/L的2甲4氯钠残留对大薸的生长均有一定的抑制作用,但短期内不能致死。当水体除草剂残留降低至田间常规管理施用浓度的1/8时,即丁草胺0.53 mg/L、苄嘧磺隆0.01 mg/L、2甲4氯钠0.42 mg/L,大薸植株形态的药害影响已经明显减轻。(2)苄嘧磺隆水体残留大于0.01 mg/L时大薸干物质产量显著降低,分株生长受到严重抑制。丁草胺残留浓度为0.53 mg/L时促进大薸干物质积累和分株生长,当残留浓度大于1.06 mg/L时大薸干物质积累和分株生长受到抑制。2甲4氯钠残留浓度低于3.36 mg/L对大薸的干物质产量、分株数及植株含水率影响一般。     

茎叶处理除草剂混配对双稃草和乱草的联合作用

近年来,双稃草和乱草在稻田的发生程度与抗药性均呈加重趋势。为有效防除这两种杂草,在温室盆栽试验中采用茎叶喷雾法施药,测定了经敌稗、噁唑酰草胺、氯氟吡氧乙酸混施处理后双稃草和乱草的鲜重,并用Colby法判断药剂间的相互作用类型。结果表明,3种除草剂混用防除双稃草时以增效作用为主,防除乱草时则以相加作用为主;在田间可考虑使用有效成分用量为敌稗1 020～2 040 g/hm²+噁唑酰草胺60 g/hm²+氯氟吡氧乙酸30～60 g/hm²的组合处理。     

三种除草剂对大型溞Daphnia magna存活、生长和繁殖的影响

为了制定除草剂在水环境中的允许浓度和排放标准,参照美国公共卫生协会等编著的《水和废水标准检验法》以及我国制定的大型溞Daphnia magna毒性测定方法,进行了丁草胺、吡嘧磺隆、苄嘧磺隆 3种稻田常用除草剂对大型溞的21 d慢性毒性试验。结果发现:随着除草剂浓度的升高,大型溞的产前发育期、产幼间隔期均缩短,每胎产幼数量先增加后减少;丁草胺各浓度处理组中,内禀增长率(rm)在0.157 2~0.314 0 d-1之间,变化较大;吡嘧磺隆各个浓度组的rm相对平稳, 为0.206 6~0.276 8 d-1;大型溞在苄嘧磺隆处理组中的rm比在其他两种除草剂中的高,为0.334 1 ~0.397 1 d-1。在丁草胺处理组中,大型溞的日生殖量较少,低于吡嘧磺隆和苄嘧磺隆处理组。     

Investigation of the Mode of Action of Nematode Neuropeptides

The neuropeptide AF2 has a complex set of actions on the dorsal muscle strip of Ascaris suum, including a potentiation of the acetylcholine-stimulated muscle contraction. Caffeine at 100 μm and 5 mm inhibited this potentiation, as did 100 μm theophylline in two out of six studies. The cyclic-AMP-potentiating compounds IBMX, dibutyryl cAMP and forskolin had no effect on the AF2-induced potentiation of the acetylcholine-stimulated muscle contraction. These preliminary data suggest that the potentiating action of AF2 is not mediated by a cAMP pathway.     

厚朴病虫害种类的初步调查

采用标准地法和线路调查法,对湖北恩施市新塘乡双河厚朴基地的厚朴病虫害进行了系统调查,记录主要虫害13种,其中叶部害虫9种,枝干害虫2种,根部害虫2种。厚朴主要病害5种。藤壶蚧、厚朴枝角叶蜂和厚朴新丽斑蚜为湖北省首次报道,小绿叶蝉为厚朴新寄主记录种。同时记录了藤壶蚧的天敌6种,其中寄生小蜂2种,瓢虫4种;厚朴新丽斑蚜的天敌昆虫8种。对藤壶蚧、厚朴枝角叶蜂和厚朴苗木根腐病等重要病虫害的发生规律进行了初步调查,同时提出了防治建议。     

Effects of timing and method of application of Penicillium oxalicum on efficacy and duration of control of Fusarium wilt of tomato

The effects of timing and method of application of Penicillium oxalicum on the control of fusarium wilt of tomato were investigated. Application of P. oxalicum to tomato seedlings in seedbeds reduced disease caused by Fusarium oxysporum f.sp. lycopersici in a growth chamber by 45–49% and in glasshouse experiments by 22–69%. Disease suppression was maintained for 60–100 days after inoculation with the pathogen in the glasshouse. No disease reduction was observed in tomato plants where P. oxalicum was applied to seeds. Treatment with P. oxalicum did not affect the population of F. oxysporum f.sp. lycopersici in the rhizosphere.     

棉花黄萎病菌致病型的AFLP分析

 选用41个棉花黄萎病菌(Verticillium dahliae)代表菌系,在温室条件下,对4个棉花品种鄂荆1号(感)、中棉所12(耐)、文-5(抗)和唐棉2号(抗)进行致病性测定,结果可将供试菌系分为落叶型与非落叶型2类。选取8对AFLP引物PCR扩增的结果中,统计带型稳定、清晰且有多态性的条带,共169条作系统聚类分析,将上述菌系分为2大类,第一类为非落叶型菌系,包括10个非落叶型菌系和1个过渡菌系;第二类为30个落叶型菌系。根据聚类分析建立树状图,发现菌系与地理来源存在一定的相关性,而依据菌系致病力强弱分类则相关关系不大。选用25对EcoRⅠ和MseⅠ引物组合,对供试的41个V.dahliae进行AFLP扩增,筛选到2对引物E64(GACTGCGTACCAATTCGAC)、M53(GATGAGTCCTGAGTAACCG)和E49(GACTGCGTACCAATTCCAG)、M65(GAT-GAGTCCTGAGTAAGAG),能分别扩增出433bp和110bp2条仅为V.dahliae非落叶型菌系独有的特异片段,可将落叶型与非落叶型菌系分开,这2条特异片段被命名为EM₄₃₃和EM₁₁₀。     

Mode of action of etoxazole

The mode of action of the 2,4-diphenyl-1,3-oxazoline acaricide/insecticide etoxazole has been argued to be moulting inhibition, but experimental results supporting this hypothesis are lacking. This study investigated the effect of etoxazole on chitin biosynthesis in the fall armyworm, Spodoptera frugiperda (Smith) (Lepidoptera: Noctuidae). Etoxazole induced moulting defects in fall armyworm larvae similar, if not identical, to those caused by benzoylphenylureas, a well-known class of insecticidal chitin biosynthesis inhibitors. Furthermore, in contrast to untreated larvae, the chitin content in the integuments of larvae several days after treatment did not differ from that in freshly ecdysed individuals, thus suggesting strong chitin biosynthesis inhibition in vivo. A more detailed investigation of the inhibitory potential by incubating cultured integument pieces from larvae of S. frugiperda with [14C]N-acetyl-D-glucosamine, a radiolabelled chitin precursor, revealed I50 values of 2.95 and 0.071 microM for etoxazole and triflumuron respectively. The incorporation of radiolabel into potassium hydroxide-resistant material was inhibited by etoxazole in a dose-dependent manner. Based on these results, it is concluded that the acaricidal and insecticidal mode of action of etoxazole is chitin biosynthesis inhibition.     

青稞种子带菌检测及杀菌剂消毒处理效果

为了研究青稞种子外部和内部携带真菌情况,比较不同杀菌剂对青稞种子的带菌消毒效果和对幼苗生长的影响,为青稞种子播前包衣处理和种传真菌病害防控提供依据,采用离体平皿法对云南迪庆‘云青1号’、‘云青2号’和‘短白青稞’3个主栽品种进行带菌检测,并对种子进行拌种或浸种处理测定6种杀菌剂对种子消毒效果,分析杀菌剂对种子发芽和幼苗生长的影响。结果表明:供试青稞种子表面携带的优势菌群为青霉(Penicilliumspp.)、镰刀菌(Fusariumspp.);种子内部寄藏的真菌主要为镰刀菌、核腔菌(Pyrenophoraspp.)、附球菌(Epicoccumspp.)、丝核菌(Rhizoctoniaspp.)、链格孢(Alternariaspp.)和木霉(Trichoderma spp.)。青稞不同品种的种子表面及内部携带的真菌种类差异较大。致病性测定表明,镰刀菌对种子萌发和幼苗生长影响最大,后期出现幼苗坏死现象。45%咪鲜胺EW、75%百菌清WP、50%福美双WP对青稞种子携带真菌均有显著抑制作用和消毒效果,50%福美双WP消毒效果最优,达100%;45%咪鲜胺EW、75%百菌清WP、50%福美双WP处理对青稞种子发芽和幼苗生长均无显著影响。     

黑麦草属DNA条形码鉴定技术研究

以毒麦、田毒麦、多花黑麦草、多年生黑麦草、硬直黑麦草、高羊茅与狗牙根等禾本科的7种植物为材料,拟采用 DNA 测序、特异性位点比对、种间遗传距离测定、建立系统树等分析候选 DNA 条形码 psbA-trnH 鉴别黑麦草属常见植物的能力。实验结果表明,以 psbA-trnH 为 DNA 条形码时,建立的系统发育树能较好区分毒麦和田毒麦与其他几种植物。psbA-trnH 序列可以作为黑麦草属植物的潜在条形码。     

百合地下害虫主要种类调查及生物（源）农药筛选

调查了甘肃省临洮县为害百合的地下害虫种类, 并以主要发生为害种类为供试对象, 采用拌土法测定了几种生物（源）农药对主要害虫的室内毒力和致死中时。调查发现小云斑鳃金龟Polyphylla gracilicornis、棕色鳃金龟Holotrichia titanis为主要发生及为害种类, 不同时间发生种类存在差异, 9月份以小云斑鳃金龟幼虫发生为害为主, 发生量占地下害虫总数的66.16%, 平均种群密度为10.48头/m2, 10月份, 则以棕色鳃金龟幼虫发生为主, 发生量占地下害虫总数的96.86%, 平均种群密度为7.79头/m2, 主要取食百合根系和鳞茎, 造成根系数量减少, 鳞茎出现不规则褐色缺口或凹陷斑。药剂筛选结果表明, 1.8%阿维菌素乳油、200亿孢子/g球孢白僵菌粉剂对两种蛴螬均具有较高的杀虫活性和速效性, 药后7 d时, 校正死亡率在82.22%以上, 对小云斑鳃金龟幼虫和棕色鳃金龟幼虫的LC50分别为0.161、0.060 mg/g和5.558×107、0.362×107孢子/g, LT50分别为2.237 d（2.2 mg/g）、1.393 d（2.2 mg/g）和6.645 d（40.0×107孢子/g）、4.940 d（2.0×107孢子/g）, 这两种生物（源）农药对两种蛴螬的LC50和LT50值均略大于两种化学农药25%二嗪磷乳油、40%辛硫磷乳油处理的, 且对小云斑鳃金龟幼虫的杀虫活性均低于对棕色鳃金龟幼虫的杀虫活性, 致死中时则长于对棕色鳃金龟幼虫的致死中时。     

Effects of different temperature treatments on dormancy of sclerotia of ten isolates of Sclerotium cepivorum

The variability of dormancy of sclerotia of ten isolates ofSclerotium cepivorum was investigated. Of all isolates tested, the freshly harvested sclerotia were dormant. After drying for 48 hours the sclerotia of six isolates were able to germinate, two isolates stayed dormant and two isolates were infested by hyperparasitic fungi. After storage in soil at 5°C or 20°C, the sclerotia of the different isolates exhibited considerable differences in respect to germination capability, but all isolates showed highest germination after a treatment of 8 weeks at 20°C followed by 8 weeks at 5°C. The sclerotia of all isolates showed an increased capacity to germinate withoutAllium extracts at 10°C after pretreatment at 30°C for 28 days.     

Allelopathy of buckwheat: Assessment of allelopathic potential of extract of aerial parts of buckwheat and identification of fagomine and other related alkaloids as allelochemicals

The allelopathic potential of buckwheat ( Fagopyrum esculentum ) was investigated. Field study showed that living buckwheat reduced weed biomass compared with plots without buckwheat. Laboratory study revealed that root exudates suppressed root and shoot growth of weeds and reduced weed dry weight. Sequential partitioning of the aqueous ethanolic extract of the aerial parts of buckwheat showed that the chloroform extract caused an 80% reduction in radicle elongation of lettuce seedlings at a concentration of less than 100 p.p.m. Fagomine, 4-piperidone and 2-piperidinemethanol were isolated and identified by ¹H and ¹³C nuclear magnetic resonance from the chloroform extract. These compounds caused a 50% inhibition of radicle elongation in lettuce seedlings at concentrations of less than 100 p.p.m. These results suggest that compounds 1, 2, and 3 might act as allelochemicals and affect the growth or germination of different plant species.