以火焰光度气相色谱法测定辛硫磷在粮食中的残留方法研究

应用不同的萃取净化方法,对用辛硫磷处理的稻谷等粮种及部分加工品中的残留以火焰光度气相色谱法在两种不同的色谱分离柱上进行测定结果指出:在5%0V-101柱上和10%DC-200柱上的回收率相差不大.用60%丙酮-水溶液萃取样品后与石油醚(30-60℃)进行液-液分配,对于大米、糙米、玉米、高梁、黄豆、绿豆等上的残留测定较为适宜.大米、糙米在5%0V-101柱上的回收率分别为97.5～100和100～110.7;在10%DC-200柱上分别为85.0～115.0和80.0～91.0.只用柱层折作为净化手段,对于处理量较高的样品有较好的回收率.采用索氏提取后,再经柱层析净化,对于只用液-液分配法回收较低的稻谷、花生果和稻壳等表面粗糙的样品有较好的回收.从二种色谱柱对辛硫磷的灵敏度和最低检出量来看,5%0V-101柱比10%DC-200柱要好些,故选用前者作为今后分析用的色谱分离柱. 为了选择一种操作简易,回收效果好,经济实用的前处理方法,又实验了以上粮种分别用不同溶剂(苯、已烷、石油醚、丙酮)萃取,不经净化,浓缩后直接进气相色谱分析,结果发现苯和已烷萃取回收率在85～108%之间.石油醚与丙酮、萃取回收率低杂峰又多. 辛硫磷作为一种广普性的杀虫剂,在农业上有广泛的用途,用作贮粮防治害虫.国外作了大量的研究工作,认为是一种有效的杀虫剂.有关辛硫磷的气相色谱残留分析方法也有报导.用火焰光度气相色谱法测定贮粮中辛硫磷的残留报导甚少,为了求出辛硫磷在贮粮中消失规律,我们研究了它的分析方法.在实验中,采用M.C.Bowman气相色谱条件;对于净化方法进行了探索,找出适合于我国实验室条件的既经济又适用的方法.     

黄曲霉毒素B_1液相色谱法检测技术比较分析

从柱前衍生、柱后衍生、荧光检测、紫外检测的分离检测技术和免疫亲和柱净化、多功能净化柱净化、硅镁吸附剂净化、液液萃取净化、硅胶净化、固相萃取等前处理技术方面对粮食中黄曲霉毒素B1的液相色谱检测技术进行了比较分析.     

固相萃取—气相色谱法检测菠菜中的54种有机磷

建立了固相萃取—气相色谱法测定菠菜中的54种有机磷农药残留的方法,即用环己烷:乙酸乙酯(1∶1,V/V)提取样品中的有机磷农药,固相萃取(SPE)柱净化,用GC—FPD法对其进行检测。结果表明,54种有机磷农药在46min内分离良好,在质量浓度为0.01～1.0mg/L时的线性良好,相关系数为0.9939～0.9999;在质量分数为0.01～0.05×10-6时,外标加标法平均回收率为65%～135%;相对标准偏差为0.25%～18%;检出限为0.0065～0.15mg/L。该方法简单、准确、可靠、灵敏度高。     

全自动免疫磁珠法与免疫亲和柱法测定玉米粉中黄曲霉毒素B1的对比研究

采用全自动免疫磁珠净化与免疫亲和柱净化的前处理方法,结合超高效液相色谱法对玉米粉中黄曲霉毒素B₁进行定量检测,并对两种前处理方法结果准确性、加标回收率、检测时间进行了对比。结果表明：对玉米粉中添加不同量的黄曲霉毒素B₁标准物质,使用免疫亲和柱净化法的加标回收率在80.96%～100.42%之间,平均回收率为88.04%,标准偏差为0.052,变异系数为5.90%;使用全自动免疫磁珠净化法的加标回收率在90.00%～108.33%之间,平均回收率为100.20%,标准偏差为0.046,变异系数为4.57%。采用配对t检验评价两种净化方式对检测结果一致性的影响,结果显示t值小于理论t₍0.05(32))的值,P>0.05,结果显示这两种净化方法的差异在可接受范围内。两种方法在净化玉米粉中黄曲霉毒素B₁中可以满足实验要求。全自动免疫磁珠净化搭配使用真菌毒素全自动净化仪前处理方法可同时处理多个样品,平均一个样品净化时间小于3 min,处理时间短、实验效率更高。     

高效液相色谱-柱后衍生法检测牛奶中10种氨基甲酸酯类农药残留

通过建立固相萃取-高效液相色谱柱后衍生法,同时测定牛奶中10种氨基甲酸酯类农药(涕灭威亚砜、涕灭威砜、灭多威、3-羟基克百威、涕灭威、速灭威、克百威、甲萘威、异丙威及仲丁威)残留。样品经乙腈提取,HLB固相萃取柱净化后,采用高效液相色谱-柱后衍生法进行测定,对每种农药进行了3种不同浓度(100,200,400μg/kg)的添加回收率试验。结果表明,10种农药的回收率在70.2%~96.7%,相对标准偏差为3.37%~6.27%。试验中所建立的10种农药测定方法完全可以满足当前农药残留分析的要求。     

DON净化柱——高效液相色谱法检测粮谷中呕吐毒素

通过自制DON净化柱和高效液相色谱仪,建立了检测谷物中呕吐毒素的方法.样品经乙腈—水溶剂提取后,通过自制的DON净化柱净化,采用C18分离柱和紫外检测器测定.结果表明:样品通过乙腈—水(体积比V/V,84∶16)混合溶剂和超声20 min的提取,可大幅度提高方法回收率;呕吐毒素在0.5 mg/kg～8.0mg/kg内线性关系好,相关系数为0.999;在0.5、2.0和8.0mg/kg的加标水平下,回收率为95.1％～102.3％,相对标准偏差为1.8％～6.4％,检出限(信噪比)为50μg/kg.     

粮食中麦角甾醇含量正相液相色谱法检测

介绍了一种可准确、快速测定粮食中麦角甾醇含量的液相色谱方法.样品皂化后,用正己烷萃取麦角甾醇,不需要进一步纯化,直接上液相色谱分析.分析柱为Spherisorb硅胶柱,检测波长282 nm.方法的检出限为0.1 mg/kg,方法的回收率在95.1%～100.0%.分析的准确度评价采用微量制备技术和反相液相色谱分离技术,证明了该方法分析的结果准确可靠.     

超高效液相色谱法快速测定烟草中的吲哚乙酸和吲哚丙酸

本研究基于自主设计的集萃取、过滤和转移功能为一体的样品萃取瓶,建立了超高效液相色谱法(UPLC)测定烟草中的吲哚乙酸和吲哚丙酸的分析方法。采用ACQUITY UPLC BEH C18(2.1×50 mm, 1.7 m)色谱柱,流动相为30%乙腈(0.01 mol/L的乙酸水溶液),样品经80%的甲醇高速匀浆萃取、MCI-GEL CHP 20 P反向树脂净化和过滤后,通过UPLC-FL进行分析检测。结果表明:自主设计的样品萃取瓶可缩短前处理时间,吲哚乙酸在1.0～210 ng/m L、吲哚丙酸在1.0～240 ng/m L内均具有良好的线性关系(线性相关系数>0.999);吲哚乙酸、吲哚丙酸的检出限分别为0.20 ng/mL与0.25 ng/m L;在不同添加水平下,平均回收率在90.5%～103.8%之间,日内精密度和日间精密度均小于3.8%,具有较好的重复性。该方法能够满足烟草中吲哚乙酸和吲哚丙酸的快速、准确测定。     

凝胶渗透色谱净化烟叶有机磷、拟除虫菊酯类农药残留的研究

为确定凝胶渗透色谱（GPC）净化烟草有机磷和拟除虫菊酯农药残留的最佳收集时间,提高烟草有机磷和拟除虫菊酯农药残留的净化效果和回收率,进行了此项试验。采用添加3个浓度梯度农药标准品进行回收试验的方法,研究了烟叶中9种有机磷农药和7种拟除虫菊酯农药在GPC柱上的流出规律。结果表明,有机磷农药的最佳收集时间为26~68 min,拟除虫菊酯类农药的最佳收集时间为26~42 min。有机磷农药的回收率为80.28%~96.81%,相对标准偏差为4.44%~8.74%,拟除虫菊酯类农药回收率为76.39%~97.95%,相对标准偏差为2.69% ~7.58%。GPC净化烟草有机磷和拟除虫菊酯农药残留的最佳收集时间与国家标准GB/T 13595不同,主要是因为农药品种不同而造成的,因此最佳收集时间必须根据具体试验来确定。     

用超高效液相色谱串联质谱法同时测定谷物中12种真菌毒素

建立了简单、快速、同步测定谷物中12种常见真菌毒素的超高效液相色谱串联质谱分析方法。样品用80%乙腈水溶液振荡提取,多功能净化柱净化,Waters ACQUITY UPLCTMBEH C18色谱柱分离, 串联四极杆质谱多反应离子监测方式检测,并采用外标法定量。结果表明, 12种真菌毒素在各自的线性响应范围内线性关系良好, 相关系数均不低于0.998,12种真菌毒素的检出限为0.016~1.000 μg kg^-1,低、中、高3个加标水平的平均回收率(n = 6)为60.0%~122.4%,相对标准偏差(RSD)为0.9%~20.3%。该方法具有前处理简单、净化效果好、灵敏度高和检测速度快的优点,适用于谷物样品中多组分真菌毒素残留的分离和定量检测。     

Biological Activity and Quantification of Suspected Allelochemicals from Alfalfa Plant Parts

Autotoxicity restricts reseeding of alfalfa (Medicago sativa L.) after alfalfa until autotoxic chemical(s) breaks down or is dispersed into external environments. A series of aqueous extracts from leaves, stems, roots and seeds of alfalfa ‘Vernal’ were bioassayed against alfalfa seedlings of the same cultivar to determine their autotoxicity. The highest inhibition was found in the extracts from the leaves. Extracts at 40 g dry tissue l^?1 from alfalfa leaves were 15.4, 17.5 and 28.7 times more toxic to alfalfa root growth than were those from roots, stems and seeds, respectively. A high‐performance liquid chromatography (HPLC) analysis with nine standard compounds showed that the concentrations and compositions of allelopathic compounds depended on the plant parts. In leaf extracts that showed the most inhibitory effect on root growth, the highest amounts of allelochemicals were detected. Among nine phenolic compounds assayed for their phytotoxicity on root growth of alfalfa, coumarin, trans‐cinnamic acid and o‐coumaric acid at 10^?3 m were most inhibitory. The type and amount of causative allelochemicals found in alfalfa plant parts were highly correlated with the results of the bioassay, indicating that the autotoxic effects of alfalfa plant parts significantly differed.     

Changes in Seed Yield and Quality with Maturity in Onion (Allium cepa L., cv. 'Early Cream Gold')

Development of onion (Allium cepa L., cv. ‘Early Cream Gold’) seed under cool climate conditions in Tasmania, Australia occurred over a longer duration than previously reported, but similar patterns of change in yield components were recorded. In contrast to previous studies, umbel moisture content declined from 85 to 67 % over 57 days while seed moisture content decreased from 85 to 31 %. Seed yield continued to increase over the duration of crop development, with increasing seed weight compensating for seed loss resulting from capsule dehiscence in the later stages of maturation. Germination percentage was high and did not vary significantly from 53 to 77 days after full bloom (DAF), but mean germination time declined and uniformity of germination increased significantly over the same time period. The percentage abnormal seedlings declined with later harvest date, resulting in highest seed quality at 77 DAF. The results of this study suggest that the decision to harvest cool climate onion seed crops before capsule dehiscence will result in a loss of potential seed yield and quality.     

Location of a high-lysine gene and the DDT-resistance gene on barley chromosome 7

Summary The high-lysine gene in Risø mutant 1508 conditions an increased lysine content in the endosperm via a changed protein composition, a decreased seed size, and several other characters of the seed. The designation lys3a, lys3b, and lys3c, is proposed for the allelic high-lysine genes in three Risø mutants, nos 1508, 18, and 19. Linkage studies with translocations locate the lys3 locus in the centromere region of chromosome 7. A linkage study involving the loci lys3 and ddt (resistance to DDT) together with the marker loci fs (fragile stem), s (short rachilla hairs), and r (smooth awn) show that the order of the five loci on chromosome 7 from the long to the short chromosome arm is r, s, fs, lys3, ddt. The distance from locus r to locus ddt is about 100 centimorgans.     

Simultaneous Determination of Four Phenolic Acids in Radix Salviae Miltiorrhizae Formula Granules by QAMS

[Objectives]This study aimed to establish a QAMS(quantitative analysis of multi-components by single-marker)method for simultaneous determination of four phenol...     

Pollen and pollination experiments. III. The viability of apple and pear pollen as affected by irradiation and storage

Summary Apple and pear pollen was irradiated with doses of 0, 50, 100, 250 and 500 krad (gamma rays) and stored at 4°C and 0–10% r.h. From the in-vitro germination percentages an average LD 50 dose of about 220 krad was estimated. For both irradiated and untreated pollen a close and corresponding lineair relationship existed between germination percentage and pollen tube growth.Irradiated pollen was much more sensitive to dry storage conditions than untreated pollen, resulting in less germination and more bursting. Apparently, irradiation caused the pollen cell membrane to lose its flexibility faster than normal. Rehydration of dry-stored, irradiated pollen in water-saturated air restored germination percentages up to their initial levels. The importance of this procedure in germination trials is stressed.     

Water Extraction Process of Chinese Herbal Compound Man Gan Ning

[Objectives]To optimize the water extraction process of Chinese Herbal Compound Man Gan Ning and establish a method for its extraction and content determination...     

Present status and future strategy in breeding faba beans (Vicia Faba L.) for resistance to biotic and abiotic stresses

Progress is being made, mainly by ICARDA but also elsewhere, in breeding for resistance to Botrytis, AScochyta, Uromyces, and Orobanche; and some lines have resistance to more than one pathogen. The strategy is to extend multiple resistance but also to seek new and durable forms of resistance. Internationally coordinated programs are needed to maintain the momentum of this work.Tolerance of abiotic stresses leads to types suited to dry or cold environments rather than broad adaptability, but in this cross-pollinated species, the more hybrid vigor expressed by a cultivar, the more it is likely to tolerate various stresses.     

Optimization of Extraction Technology and Determination of Content of Total Phenols of Leaves in Acanthopanax giraldii Harms

[Objectives] To determine the optimum extraction technology for total phenols of leaves in Acanthopanax giraldii Harms.[Methods]The single factor test and ortho...     

Cytoplasmic male sterility,resistance to gall mite and mildew,and season of leafing out in black currants

Summary Cytoplasmic male sterility (cms) is described in the F₁ hybrids Ribes × carrierei (R. glutinosum albidum × R. nigrum) and R. sanguineum × R. nigrum. In backcrosses to R. nigrum, progenies with R. glutinosum cytoplasm were either all male sterile, or segregated for full male fertility (F) and complete (S) and partial (I) male sterility. Ratios of F:I+S suggested that two linked genes controlled cms, F plants being dominant for one (Rf ₁) and recessive for the other (Rf ₂).Segregation for cms in relation to three linded genes, Ce (resistance to the gall mite, Cecidophyopsis ribes), Sph ₃(resistance to American gooseberry mildew, Sphaerotheca mors-uvae) and Lf ₁(one of two dominant additive genes controlling early season leafing out) indicated that Rf ₁and Rf ₂were in this linkage group. The gene order and approximate crossover values appeared to be: % MathType!MTEF!2!1!+-% feaafiart1ev1aaatCvAUfeBSjuyZL2yd9gzLbvyNv2CaerbuLwBLn% hiov2DGi1BTfMBaeXafv3ySLgzGmvETj2BSbqef0uAJj3BZ9Mz0bYu% H52CGmvzYLMzaerbd9wDYLwzYbItLDharqqr1ngBPrgifHhDYfgasa% acOqpw0xe9v8qqaqFD0xXdHaVhbbf9v8qqaqFr0xc9pk0xbba9q8Wq% Ffea0-yr0RYxir-Jbba9q8aq0-yq-He9q8qqQ8frFve9Fve9Ff0dme% aabaqaciGacaGaamqadaabaeaafaaakeaacaWGdbGaamyzamaamaaa% baGaaiiiaiaacccacaGGWaGaaiOlaiaacgdacaGG0aGaaiiiaiaacc% caaaGaaiiiaiaacccacaGGGaGaamOuaiaadAgaliaaigdakmaamaaa% baGaaiiiaiaacccacaGGGaGaaiiiaiaaccdacaGGUaGaaiOmaiaacs% dacaGGGaGaaiiiaiaacccacaGGGaGaaiiiaaaacaWGsbGaamOzaSGa% aGOmaOWaaWaaaeaacaGGGaGaaiiiaiaacccacaGGGaGaaiiiaiaacc% cacaGGGaGaaiiiaiaacccaaaGaamitaiaadAgaliaaigdakmaamaaa% baGaaiiiaiaacccacaGGGaGaaiiiaiaacccacaGGGaGaaiiiaiaacc% cacaGGGaGaaiiiaiaacccacaGGGaaaaiaadofacaWGWbGaamiAaSGa% aG4maaaa!6E4D!\[Ce\underline { 0.14 } Rf1\underline { 0.24 } Rf2\underline { } Lf1\underline { } Sph3\]. Crossover values of 0.36 for Ce-Lf ₁, and 0.15 for Lf ₁-Sph ₃were estimated from the relative mean differences in season of leafing out between seedlings dominant and recessive for Ce and Sph ₃.It is suggested that competitive disadvantage of lf ₁-carrying gametes and/or zygotes at low temperatures may be implicated in the almost invariable deficit of plants dominant for the closely linked mildew resistance allele Sph ₃. Poor performance of lf ₁- (and possibly lf ₂-) carrying gametes and young zygotes during periods of low temperature at flowering might also account for the liability of some late season cultivars and selections to premature fruit drop (running off).     

Screening techniques and sources of resistance to parasitic angiosperms

Parasitic angiosperms cause great losses in many important crops under different climatic conditions and soil types. The most widespread and important parasitic angiosperms belong to the genera Orobanche, Striga, and Cuscuta. The most important economical hosts belong to the Poaceae, Asteraceae, Solanaceae, Cucurbitaceae, and Fabaceae. Although some resistant cultivars have been identified in several crops, great gaps exist in our knowledge of the parasites and the genetic basis of the resistance, as well as the availability of in vitro screening techniques. Screening techniques are based on reactions of the host root or foliage. In vitro or greenhouse screening methods based on the reaction of root and/or foliar tissues are usually superior to field screenings and can be used with many species. To utilize them in plant breeding, it is necessary to demonstrate a strong correlation between in vitro and field data. The correlation should be calculated for every environment in which selection is practiced. Using biochemical analysis as a screening technique has had limited success. The reason seems to be the complex host-parasite interactions which lead to germination, rhizotropism, infection, and growth of the parasite. Germination results from chemicals produced by the host. Resistance is only available in a small group of crops. Resistance has been found in cultivated, primitive and wild forms, depending on the specific host-parasite system. An additional problem is the existence of pathotypes in the parasites. Inheritance of host resistance is usually polygenic and its transfer is slow and tedious. Molecular techniques have yet to be used to locate resistance to parasitic angiosperms. While intensifying the search for genes that control resistance to specific parasitic angiosperms, the best strategy to screen for resistance is to improve the already existing in vitro or greenhouse screening techniques.