毛细管气相色谱法测定苹果中氯氟氰菊酯残留

建立了苹果中氯氟氰菊酯残留量的乙腈提取、弗罗里硅土(Florisil)层析净化、毛细管气相色谱-电子捕获检测器测定方法,对苹果中的氯氟氰菊酯残留进行了测定。本研究对苹果样品中农药残留提取采用乙腈代替传统的丙酮-石油醚作为提取剂,提取率高,提取溶液干净。通过Florisil层析柱净化,毛细管气相色谱—电子捕获检测器测定,既节省了溶剂用量、时间,又简化了预处理步骤。隔垫吹扫和玻璃衬管内填充玻璃棉消除了因样品蒸发的反扩散、吸附和垫片流失所造成的色谱峰拖尾和鬼峰的干扰。本方法得到的苹果全果、果皮和果肉中氯氟氰菊酯添加回收率分别达到92.54%±2.3%~103.32%±4.4%、96.00%±2.8%~101.23%±2.9%和92.50%±3.6%~104.02%±2.9%;氯氟氰菊酯的最小检出限为5.70×10-11g,方法简单、快速,且回收率和灵敏度高,变异系数小。     

马铃薯及土壤中丙炔噁草酮的气相色谱残留分析方法

建立了测定马铃薯及土壤中丙炔噁草酮及其代谢物RP017272和RP025496残留的气相色谱检测方法。植株、块茎样品以乙腈作为提取溶剂,土壤以二氯甲烷作为提取溶剂,选用KB-5（30m×320m×0.33m）色谱柱分离,电子捕获检测器定量检测丙炔噁草酮及其代谢物。该方法丙炔噁草酮及其代谢物的最小检出量均为5×10-12g,丙炔噁草酮、RP017272、RP025496的线性相关系数分别为0.999 2、0.998 6、0.997 2。丙炔噁草酮在马铃薯植株、块茎及土壤中的加标回收率为90.6-96.7%,相对标准偏差（RSD）为1.1-2.4%,RP017272和RP025496在土壤中的加标回收率为88.1-95.4%,相对标准偏差（RSD）为1.5-3.3%。方法具有简便、快捷,准确的特点,适合马铃薯植株、块茎及土壤中丙炔噁草酮及其代谢物残留量的测定。     

土壤中吡唑醚菌酯的残留分析方法和消解动态研究

对吡唑醚菌酯在土壤中的残留分析方法进行探讨,采用乙腈提取、Flolisil小柱净化、GC-μECD进行检测。结果表明：土壤中添加标准品0.02,0.2和1μg/g,回收率为93.0%,82.5%和83.1%。北京田间试验得到的吡唑醚菌酯在土壤上的消解动态方程为wt=w0×exp（-0.036 4t）,半衰期为19.0d。本方法灵敏度、准确度、精密度高,仪器耗材普遍易得,能够为大规模监测吡唑醚菌酯的残留情况提供参考。     

板兰根中三种拟除虫菊酯杀虫剂的残留分析

研究了板蓝根中3种拟除虫菊酯杀虫剂残留分析方法。以石油醚为萃取溶剂，分别用索氏抽 提法、浸渍振荡法、超声波法提取。提取液经100 mL丙酮∶0.05 mol/L氯化钙溶液(1∶1)液 -液分配净化后，以弗罗里硅土柱净化，5%乙酸乙酯-石油醚淋洗，气相色谱法电子捕获检 测器测定。结果表明，方法的线性范围为0.4×10-10～4×10-10g，氯氰菊酯 、氰戊菊酯、溴氰菊酯最低检测浓度分别为5×10-3、5×10-3、2×10-3 mg/kg。3种提取方法对板蓝根的添加回收率、变异系数符合农药残留分析的要求。     

HPLC/MS/MS测定铁皮石斛中咪鲜胺残留

用高效液相色谱-质谱联用法定量检测铁皮石斛中的咪鲜胺残留,用乙腈提取铁皮石斛植株中的残留咪鲜胺,分析色谱柱为C_(18)(100mm×2.1mm×2.6μm),以甲醇和乙酸铵溶液梯度洗脱,采用选择离子监测模式,以保留时间和质荷比对咪鲜胺予以定性确认,以m/z=308.07为检测定量离子。咪鲜胺出峰时间在3.87min左右,方法检出限为0.52μg/kg,平均回收率在89.2%~114.7%之间。该方法灵敏、准确、定量范围宽、耐用性强,可作为铁皮石斛中咪鲜胺残留的可靠检测方法 。     

水稻中乙酰甲胺磷及其代谢产物甲胺磷农药残留分析方法

采用乙腈和水（70：5,V／V）为溶剂提取水稻中乙酰甲胺磷、甲胺磷,其他采用NY/T761—2008方法,气相色谱法（FPD检测器）进行测定2种农药在糙米中的残留,其添加回收率为78．7％-91．8％,变异系数为5．72％-14．1％,乙酰甲胺磷的最低检出限为0．005mg/kg,甲胺磷的最低检出限为0．01mg／kg。     

三甲苯草酮溶液稳定性研究

初步研究了三甲苯草酮在不同溶剂和不同温度下的溶液稳定性。三甲苯草酮标样经乙腈、甲醇和V (乙腈) : V (2%乙酸水溶液) = 80 : 20的混合溶剂溶解后,分别在25 ℃、40 ℃和60 ℃条件下恒温水浴,24 h内多点取样,样品经超高效液相色谱-串联质谱仪 (UPLC-MS/MS) 定性分析,高效液相色谱-二极管阵列检测器 (HPLC-DAD) 定量分析,通过分析三甲苯草酮异构体比例和噁唑重排产物转化率,对溶液的稳定性进行了评估。结果表明:烯醇式E-三甲苯草酮和Z-三甲苯草酮存在异构化现象,其中前者为优势构象;三甲苯草酮在溶液中的稳定性与溶剂种类和温度密切相关。本研究中,在极性较低的乙腈溶剂中三甲苯草酮稳定性较好;在极性较高的甲醇和V (乙腈) : V (2%乙酸水溶液) = 80 : 20混合溶剂中,存在E-三甲苯草酮向Z-三甲苯草酮转化现象,并很快达到平衡,同时可经贝克曼重排生成1,3-噁唑重排产物,且高温和高极性溶剂都有利于噁唑重排产物的生成。研究表明,极性较低的乙腈适宜作为三甲苯草酮的储备液溶剂和流动相,且低温环境有利于提高三甲苯草酮溶液的稳定性。     

菠菜中3种新烟碱杀虫剂多残留分析方法研究

研究确立了以乙腈为分散萃取溶剂,以羧基化双壁碳纳米管(DWCNTs-COOH)和石墨化碳黑(GCB)为基质分散材料的菠菜样品中呋虫胺、烯啶虫胺和吡虫啉残留的基质分散萃取前处理方法,建立并优化了乙腈梯度洗脱的高效液相色谱(HPLC)残留样品外标定量方法。结果表明,优化色谱条件下,呋虫胺、烯啶虫胺和吡虫啉色谱保留时间分别为6.8、8.6和17.7min,在0.025~25.00mg/L范围内与对应色谱峰面积具有良好的线性关系。呋虫胺、烯啶虫胺和吡虫啉在菠菜中3个添加水平的回收率均在75%以上,相对标准偏差均小于10%,该色谱条件下方法的最低检测浓度分别为0.091 2mg/L(呋虫胺)、0.080 8mg/L(烯啶虫胺)和0.062 8mg/L(吡虫啉),表明研究建立的残留样本前处理方法和样品检测方法简便、高效、经济、可靠,可满足3种农药在菠菜中残留的定量检测要求。     

高效液相色谱法测定马铃薯和土壤中的氰霜唑残留

利用高效液相色谱法研究马铃薯和土壤中氰霜唑残留的分析方法,该方法具有快速、准确、灵敏度高等特点。样品用乙腈提取,提取液经固相萃取小柱净化,高效液相色谱(VWD)测定。结果表明,该方法对马铃薯和土壤中氰霜唑的最低检出浓度为4.0×10-2mg/kg。回收率在85.86%~98.99%之间,变异系数在2.06%~4.52%。     

葡萄及土壤中咪鲜胺锰盐50%可湿性粉剂高效液相色谱分析方法研究

研究咪鲜胺在葡萄及土壤中残留分析方法。样品经过盐酸乙腈提取,用SPEFlorisil柱净化,高效液相色谱测定。咪鲜胺最小检出量1.0×10-10g,最低检出浓度葡萄中为0.04mg/kg,土壤中为0.05mg/kg。咪鲜胺在葡萄、土壤中的平均回收率分别为85.9%~87.4%、83.3%~92.2%,标准偏差分别为2.0%~7.9%、2.9%~6.3%,变异系数分别为2.3%~9.2%、3.2%~7.5%。该方法操作简便、准确可靠、重复性好、速度快,符合农药残留量的分析与检测要求,适用于实际样品中咪鲜胺残留检测。     

Dermestid beetles in ‘evolution Canyon’, lower Nahal Oren, Mt. Carmel, including new records for Israel

Fifteen species of dermestid beetles were recorded at ‘Evolution Canyon’ (EC), Lower Nahal Oren, Mt. Carmel, Israel. They represent ~35% of known Israeli dermestid species. The following three species were recorded for the first time in Israel:Trogoderma svriaca Dalla Torre, 1911;Ctesias svriaca Ganglbauer, 1904; andAnthrenus (s.str.) jordaniens Pic, 1934. Adults of 13 species were collected on the more solar radiated, warmer and climatically more fluctuating south-facing slope (SFS); ten species were collected on the opposite, north-facing slope (NFS), which was cooler and climatically more stable. The abundance of adult dermestid beetles was 1.9 times higher on the SFS than on the NFS (86 and 47, respectively). Species richness and abundance distribution at EC (three collecting stations on each slope and one at the valley bottom) were significantly negatively correlated with the plant cover that consisted of trees and bushes (Spearmanr _s ,P=0.007 and 0.039, respectively) and perennials (Spearmanr _s ,P=0.039 and 0.077, respectively), indicating that non-woody plants were preferred by adult dermestid beetles.     

Epidemiology of Toxigenic Fungi and their Associated Mycotoxins for Some Mediterranean Crops

Recent data on the epidemiology of the common mycotoxigenic species of Fusarium, Alternaria, Aspergillus and Penicillium in infected or colonized plants, and in stored or processed plant products from the Mediterranean area are reviewed. Emphasis is placed on the toxigenicity of the causal fungal species and the natural occurrence of well known mycotoxins (aflatoxins, ochratoxins, fumonisins, trichothecenes, zearalenone, patulin, Alternaria-toxins and moniliformin), as well as some more recently described compounds (fusaproliferin, beauvericin) whose toxigenic potential is not yet well understood. Several Fusarium species reported from throughout the Mediterranean area are responsible of the formation of mycotoxins in infected plants and in plant products, including: Fusarium graminearum, F. culmorum, F. cerealis, F. avenaceum, F. sporotrichioides and F. poae, which produce deoxynivalenol, nivalenol, fusarenone, zearalenone, moniliformin, and T-2 toxin derivatives in wheat and other small grains affected by head blight or scab, and in maize affected by red ear rot. Moreover, strains of F. verticillioides, F. proliferatum, and F. subglutinans, that form fumonisins, beauvericin, fusaproliferin, and moniliformin, are commonly associated with maize affected by ear rot. Fumonisins, were also associated with Fusarium crown and root rot of asparagus and Fusarium endosepsis of figs, caused primarily by F. proliferatum. Toxigenic A. alternata strains and associated tenuazonic acid and alternariols were commonly found in black mould of tomato, black rot of olive and citrus, black point of small cereals, and black mould of several vegetables. Toxigenic strains of A. carbonarius and ochratoxin A were often found associated with black rot of grapes, whereas toxigenic strains of A. flavus and/or P. verrucosum, forming aflatoxins and ochratoxin A, respectively, were found in moulded plant products from small cereals, peanuts, figs, pea, oilseed rape, sunflower seeds, sesame seeds, pistachios, and almonds. Finally, toxigenic strains of P. expansum and patulin were frequently found in apple, pear and other fresh fruits affected by blue mould rot, as well as in derived juices and jams.     

A survey of the genera of<Emphasis Type="Italic">Microgaster</Emphasis> latreille and<Emphasis Type="Italic">Hygroplitis</Emphasis> thomson (Hymenoptera: Braconidae: Microgastrinae) from China

The genera ofMicrogaster Latreille 1804 andHygroplitis Thomson 1895 from China are presented systematically in this paper. Thirty-two species ofMicrogaster and three species ofHygroplitis are known in China. Diagnosis, character variation, distribution and host of each species among the two genera are presented, including its host and distribution. Keys to the species ofMicrogaster andHygroplitis are given. http://www.phytoparasitica.org posting Dec. 19, 2006.     

Plant Viruses Transmitted by Whiteflies

One-hundred and fourteen virus species are transmitted by whiteflies (family Aleyrodidae). Bemisia tabaci transmits 111 of these species while Trialeurodes vaporariorum and T. abutilonia transmit three species each. B. tabaci and T. vaporariorum are present in the European–Mediterranean region, though the former is restricted in its distribution. Of the whitefly-transmitted virus species, 90% belong to the Begomovirus genus, 6% to the Crinivirus genus and the remaining 4% are in the Closterovirus, Ipomovirus or Carlavirus genera. Other named, whitefly-transmitted viruses that have not yet been ranked as species are also documented. The names, abbreviations and synonyms of the whitefly-transmitted viruses are presented in tabulated form together with details of their whitefly vectors, natural hosts and distribution. Entries are also annotated with references. Whitefly-transmitted viruses affecting plants in the European–Mediterranean region have been highlighted in the text.     

Broad bean mottle virus in Morocco; curculionid vectors,and natural occurrence in food legumes other than faba bean (Vicia faba)

Broad bean mottle virus (BBMV) was transmitted from infected to healthy faba-bean plants by the curculionid weevilsApion radiolus Kirby,Hypera variabilis Herbst,Pachytychius strumarius Gyll,Smicronyx cyaneus Gyll, andSitona lineatus L. The latter appeared to be an efficient vector: acquisition and inoculation occurred at the first bite, the rate of transmission was c. 41%, and virus retention lasted for at least seven days.S. lineatus transmitted the virus from faba bean to lentil and pea, but not to the three genotypes of chickpea tested. This is the first report on the generaHypera, Pachytychius, andSmicronyx as virus vectors, and onA. radiolus, H. variabilis, P. strumarius, andS. cyaneus as vectors of BBMV.Out of 351 samples of food legumes with symptoms suggestive of virus infection, 16, 11, 19, and 17% of the samples of chickpea, lentil, pea, and common bean, respectively, were found infected when tested for BBMV in DAS-ELISA. This is the first report on the natural occurrence of BBMV in chickpea, lentil, pea, and common bean. The virus should be regarded as a food-legume virus rather than a faba-bean virus solely, and is considered an actual threat to food legume improvement programmes.     

Characterization of potato potyvirus Y (PVY) isolates from seed potato batches. Situation of the NTN, Wilga and Z isolates

A collection of 38 PVY isolates from seed potato batches, originating from several Western European countries, was characterized by using current biological, serological and molecular tools differentiating PVY strains and groups. The correlation between the three kinds of tests was good but not absolute. No single serological or PCR method was able to discriminate among the five isolate groups found. Twenty-nine isolates belonged to the PVY^N strain and six to the PVY^O strain. No PVY^C was found. Two other isolates reacted serologically like PVY^O, but were unable to elicit a hypersensitive response from the Ny_tbr gene and probably represent the PVY^Z group. At the molecular level, these two isolates showed a combination of both PVY^O and PVY^N and could be recombinants of these strains. Another isolate reacted serologically like PVY^O, but induced vein necrosis in tobacco, like PVY^N-Wilga. Some PVY^N isolates caused tuber ring necrosis in glasshouse conditions. These might belong to the PVY^NTN group. The PVY^NTN, PVY^N-Wilga and PVY^Z groups probably represent pathotypes within strains PVY^N and PVY^O, respectively. The present study also confirms previous reports showing a high genetic variation at the 5 end within the PVYN strain.     

The autumn leafroller: Phenology,damage and parasitoids in a Dutch apple orchard

The phenology of the autumn leafroller,Syndemis musculana, a local pest of apple, was studied in order to forecast larval emergence. From 1983–1986, peak flight as determined with sexpheromone traps was always between 13–18 May. The duration of embryonic development was determined at various constant temperatures and used to estimate the periods of egg hatch in these four years. Each year, most eggs should have hatched in the second decade of June.Differences in attack rates between apple cultivars seem to be explained largely by the variation in picking time. Larvae are only half grown at the beginning of harvest (cv. James Grieve), and have gone into hibernation when the latest variety (cv. Golden Delicious) is picked. Moreover, the varieties Cox's Orange Pippin and Belle de Boskoop, picked about half time, are liable to receive additional damage by caterpillars brought with the picked fruits into storage.Various hymenopterous parasites were reared from caterpillars. As the only leafroller in the orchard which hibernates as mature larva,S. musculana may promote winter survival of some parasitoids, like the eulophidColpyclypeus florus.Samenvatting De fenologie van de herfstbladroller (Syndemis musculana Hübner), een incidentele plaag op appel, werd nader bepaald met het doel het uitkomen van de eieren te kunnen voorspellen. In 1983–1986 viel de piekvlucht, bepaald met behulp van feromoonvallen, steeds tussen 13 en 18 mei.De ontwikkelingsduur van de eieren bij verschillende constante temperaturen werd gebruikt om de periode van uitkomen te schatten. De meeste eieren zullen ieder jaar in de eerste helft van juni uitkomen.Geconstateerde verschillen in schade tussen appelrassen blijken goeddeels terug te voeren op verschillen in pluktijdstip. De rupsen van de herfstbladroller zijn pas half-was als de eerste appels eind augustus geplukt worden, terwijl tegen het einde van de oogst begin oktober de meeste al in winterslaap zijn. Met name tussentijdse rassen, als Cox's Orange Pippin and Schone van Boskoop, lopen extra schade op doordat grotere rupsen met de geplukte vruchten in de kist terecht komen.Uit de rupsen werden negen, al van andere boomgaardbladrollers bekende, sluipwespen gekweekt, Omdat deze bladrollersoort, als enige in de boomgaard, als volgroeide rups overwintert, lijkt zij bij uitstek geschikt als winterwaard.This study was carried out at the Experimental Orchard De Schuilenburg, Schuilenburg 3, 4041 BK Kesteren, the Netherlands, to which address correspondence should be addressed.     

Characterization of Sclerotinia minor populations in Texas peanut fields

In the summer of 2004 an epidemic of sclerotinia blight of peanut, a disease caused by Sclerotinia minor, occurred in Texas in fields where the disease was never previously detected. The disease was observed on many plants within one of the fields (>3000 disease foci), although most foci were <1 m. It is hypothesized that these observations were inconsistent with the recent introduction of a monocyclic pathogen, even if disease developed under conducive environmental conditions. The pattern of disease is most suggestive of the presence of foliar (ascospore) infections, although air temperature was above the known limits for apothecia development if the pathogen had arrived in the field in 2004 peanut seed. To further examine this epidemic, 232 isolates were collected, across a variety of spatial scales spanning this field and other Texas peanut fields, and evaluated for aggressiveness, fungicide sensitivity and genotypic diversity. There was wide variation among isolates for the phenotypic characteristics measured, but there was no evidence that a genotypically unique, highly aggressive, and fungicide resistant isolate had been introduced or evolved. The predominant genotype, TX1, which contained 154 isolates, was found in every county and field population.     

Tumours of Begonia and some other ornamentals,induced by Corynebacterium fascians

In 1975 many tumours were observed in plants ofBegonia Schwabenland grown in Aalsmeer. Submersion of the roots ofNicotiana megalosiphon seedlings in a homogenate of tumorous tissue, induced tumours after two weeks. Short periods of submergence yielded results similar to those obtained after longer periods. Tumour homogenates lost their infectivity after ten min at 50°C. Aphids transmitted the infectious agent.Treatment with propylene oxide did not inhibit infectivity completely. Filtration through a 450 nm filter removed the infectious agent.Tobacco tumor virus or a viroid could not be isolated. Cultures ofCorynebacterium fascians, isolated from tumours ofN. megalosiphon were highly infectious and induced tumours in healthyN. megalosiphon andBegonia. Tumorous tissue homogenates ofPelargonium zonale, Dahlia sp.,Gladiolus sp., andLilium sp. also caused tumours inN. megalosiphon, from whichC. fascians was isolated. It was not possible to produce tumours inN. megalosiphon with homogenates from roses with symptoms of bud proliferation.Samenvatting In 1975 werden vele tumoren waargenomen inBegonia Schwabenland op Aalsmeerse bedrijven (Fig. 1). De infectiositeit van tumorweefsel kon goed en snel worden vastgesteld door de wortels van zaailingen vanNicotiana megalosiphon in een homogenaat van tumorweefsel te dompelen. Tumoren ontstonden na twee weken, de eindbeoordeling geschiedde na een maand (Fig. 2). Ook verschillende andereNicotiana spp.,Melilotus officinalis (Fig. 3) enPisum odoratum (Fig. 4) werden aangetast.Bij de infectiositeitstoets gaven zeer korte dompeltijden even goede resultaten als langere (Tabel 1). Infectieus sap verloor zijn infectievermogen na 10 min verhitting bij 50°C. Bladluizen brachten de smetstof over. Propyleenoxide verminderde de infectiositeit wel, doch onderdrukte deze niet totaal. Bij filtratie door een 450 nm filter bleef het infectieuse agens op het filter achter. Het tumor-inducerende agens was ook aanwezig in die delen van planten met tumoren welke gezond leken en het ging voor een gering deel over met zaad (Tabel 2).Uit tumoren konden wij geen tabakstumorvirus of een viroïde isoleren. Culturen vanCorynebacterium fascians, geïsoleerd uit tumoren vanN. megalosiphon bleken zeer infectieus en veroorzaakten tumoren inN. megalosiphon enBegonia. Homogenaten van tumorweefsel vanPelargonium zonale, dahlia (Fig. 5), gladiool (Fig. 6) enLilium Mid Century Hybrid Enchantment (Fig. 7) veroorzaakten ook tumoren opN. megalosiphon, waaruitC. fascians werd geïsoleerd. Met sap van kroeskopzieke rozen konden wijN. megalosiphon niet besmetten.     

Eyespot of Cereals Revisited: ITS phylogeny Reveals New Species Relationships

Four species so far classified in Pseudocercosporella or Ramulispora (hyphomycetes) are associated with eyespot disease symptoms of cereals. Two of these have been linked to teleomorphs that were described in Tapesia. Sequence data derived from the Internal Transcribed Spacer region (ITS1, 5.8S and ITS2) of the rDNA operon showed, however, that the eyespot fungi associated with Tapesia are not congeneric with Ramulispora sorghi, the type of Ramulispora. The genus name Tapesia is now rejected in favour of the conserved name Mollisia, which appears to comprise heterogeneous fungi. Tapesia yallundae is not closely related to the type of Mollisia, M. cinerea, but clusters separately, being more closely allied to species with Cadophora anamorphs. A new holomorph genus, Oculimacula, is therefore proposed for teleomorphs of the eyespot fungi, while the anamorphs are accommodated in Helgardia gen. nov.