大型仪器作为高等学校的优质资源,在高等学校教学中发挥着越来越重要的作用.大型仪器为教学服务主要体现在,为本科生的实验教学和学校的科研工作提供技术服务.对于本科教学,主要目的是使学生掌握仪器的工作原理、操作技能和数据分析方法;对于科研工作,则以科研人员为主要对象,举办技术培训和技术讲座.适当的教学方法和合理的实验安排,能增加教学的趣味性,调动学生学习大型仪器使用的热情和积极性,有利于学生综合素质的培养.同时,应重视仪器管理人员知识更新和继续教育的诉求,在教学安排上注重理论教学和实验教学相结合,从而实现二者相互促进.

榆跳象(Orchestes alni Linnaeus)是一种危害榆树叶片的毁灭性害虫,成虫和幼虫均危害榆树叶片.采用有机溶剂浸提法在4—6月分3次获得榆跳象雌性成虫性信息素的粗提取物,并分别通过气相色谱-质谱联用仪进行分析.结果表明,4—6月份的性信息素疑似物分别有5,6,6个.通过与鳞翅目及鞘翅目象甲科等昆虫性信息素比较,并基于多数昆虫性信息素的共同特征,最终确定2种性信息素疑似组分,即11,13-二甲基-12-乙酸酯、顺-9-十四碳烯酸异丁酯.该研究初步明确榆跳象雌性成虫性信息素的主要成分,可为下一步性信息素的合成和林间诱捕实验提供参考.

速灭威是枸杞中常用的一种氨基甲酸酯类农药,在防治枸杞蚜虫的同时,残留在枸杞和土壤中的农药又会对生态环境造成危害.通过田间试验,研究了速灭威在枸杞和土壤中的残留与消解动态.结果表明,速灭威在枸杞和土壤中的半衰期分别为3.38 d和5.29 d.将25％ 速灭威可湿性粉剂以750 g·hm-2和1500 g·hm-2剂量在枸杞上施药,喷施药2～3次,施药间隔期7 d,距最后一次施药21 d,速灭威在枸杞和土壤中的最大残留量分别为0.0485 mg·kg-1和0.1596 mg·kg-1.建议速灭威在枸杞上的最大允许残留限量为0.05 mg·kg-1,施药安全间隔期为21 d.

采用Fenton法对水中几种氨基甲酸酯类农药(速灭威、克百威和抗蚜威)进行降解,考察了时间、FeSO4·7H2 O用量、H2 O2体积等因素对农药降解率的影响.结果 表明,时间、FeSO4·7H2 O用量、H2 O2用量对三种农药的降解具有重要影响,随着时间的增加,三种农药的降解率逐渐增加,在2h内降解速度最快,之后逐渐趋于平缓;当FeSO4·7H2 O用量<1 g时,三种农药的降解率随着FeSO4·7H2 O用量的增加而增加;三种农药的降解率随着H2 O2体积的增加而逐渐增加,当H2 O2体积为6 mL时,三种农药的降解率都达到90％以上.在优化的实验条件下,三种农药的降解率分别为速灭威95.5％,克百威98.9％,抗蚜威93.5％.

应用薄层层析法和柱淋洗法研究了速灭威在3种枸杞产区土壤——灌淤土、灰钙土和潮土中的迁移及淋溶特性,并探讨了土壤类型、pH值、淋溶量等因素对其淋溶的影响.结果表明:速灭威在三种枸杞产区土壤中的移动性由大到小依次为:灰钙土>潮土>灌淤土,比移值Rf分别为0.47、0.37和0.35,移动速率m/(cm·h–1/2)分别为3.52、2.58和2.35.速灭威在三种土壤中的比移值Rf在0.35—0.64之间,属于中等移动农药.速灭威在三种土壤中的淋出率由大到小依次为:潮土>灰钙土>灌淤土,淋出率分别为63.1％、50.0％和28.3％.随着水量的增加,速灭威在三种土壤中的淋溶率也越来越大.当淋溶水量大于350 mL时,除潮土外,灌淤土和灰钙土中几乎无速灭威流出,进一步证明了速灭威可能在潮土中的吸附力较低,而在灌淤土和灰钙土中的吸附力较高.淋溶液pH值不同,淋溶率也有较大差异,在灌淤土和灰钙土中弱酸性条件利于速灭威淋出,在潮土中性条件易于淋出,这可能与土壤的pH及全盐量含量不同有关,在弱酸性条件下,潮土的全盐量含量高,增大了对速灭威的吸附力,导致速灭威的淋溶率降低.速灭威在土壤中属于中等移动农药,对地下水存在一定的危险.

速灭威是枸杞中常用的一种氨基甲酸酯类农药,在防治枸杞蚜虫的同时,残留在土壤中的速灭威又会经淋溶作用渗透到地下水中,对地下水造成严重的威胁.文章采用臭氧发生器对臭氧/双氧水(O3/H2O2)降解水中速灭威进行了试验研究,考察了O3流量、pH、氧化时间等因素对速灭威降解率的影响,并采用气相色谱与质谱联用仪(GC-MS)对降解后的产物进行分析,探讨O3/H2O2降解速灭威可能的反应机理.结果 表明:(1)pH为6时,降解率最大,为44％,而在中性条件下降解率最低;(2)随着臭氧流速的增加,速灭威的降解率也逐步增加,当臭氧流速为0.6 L/min时速灭威全部降解;(3)随着时间的延长,速灭威的降解率逐渐增加,其中,在1 h内降解迅速,2h时速灭威已经100％降解;(4)降解得到的中间产物主要有间甲基苯酚等,据此推断降解机理可能是·OH自由基断裂醚键,推导了O3/H2O2氧化速灭威可能的降解途径.

Lycium barbarum is a valuable traditional Chinese medicine. Ningxia is the origin of Lycium barbarum. M-tolyl methylcarbamate (MTMC) is a commom carbamate pesticide. In this paper, at first, batch equilibrium experiments were used to investigate the adsorption and desorption of MTMC in three soils such as irrigation silting soil, fluvo-aquic soil and sierozem in Lycium barbarum field.Several models such as Freundlich,Langmuir and Linear and different thermodynamic functions such as free enthalpy(?G), enthalpy(?H) and entropy(?S) calculated by Gibbs equation were used to characterize the adsorption and desorption, and calculate distribution coefficients. The result was investigated by dynamic experiment that the adsorption capacity reached maximum value after 10 h, in order to ensure that MTMC was completely adsorbed onto soils, the time of equilibrium adsorption was set 24 h. Meantime, the desorption capacity of MTMC began to flatten after 12 h, while the maximum desorption capacity was close to 12 μg·g-1, which was much smaller than adsorption capacity, it was proved that the adsorption was nearly irreversible. Secondly, the result by isothermal adsorption experiment showed that adsorption data could be best described by the Freundlich model, the adsorption abilities of different soils were as follows: sierozem>irrigation silting soil>fluvo-aquic soil with the Kfvalue of 338.84, 234.42 and 218.78, individually, while desorption data could be best described by Langmuir model, the desorption abilities of different soils were as follows: irrigation silting soil> sierozem>fluvo-aquic soil with the Kdvalue of 389.50, 264.85 and 202.51, individually. Moreover, the average hysteresis index (HIa) was less than zero, which improved that adsorption-desorption was insignificant, and MTMC could migrate quickly in soils. Finally, the result by thermodynamics calculation showed that ?H<0,and?S>0 for irrigation silting soil and sierozem showed that electrostatic force played an important role. While for fluvo-aquic soil,?H>0,and ?S>0 identified that hydrophobic force played an important role. The result of this paper could provide a certain reference to guarantee the quality of Lycium barbarum and preserve the origin environment.

采用气相色谱-质谱联用(GC-MS)建立了对枸杞(Lycium barbarum L.)中6种有机磷农药快速测定方法.采用全扫描方式(SCAN)确定保留时间,离子扫描(SIM)模式进行定量,结合总离子流图,分别对离子源温度、进样口温度和接口温度进行优化.结果表明,离子源温度200℃,进样口温度220℃,接口温度250℃,升温程序条件为初始温度80℃,以10 ℃/min的速度升温至200℃,再以20℃/min升温至280℃,保持2min,分析检测时间控制在18 min内,达到快速、准确的检测要求.

[目的]建立基质固相分散净化、高效液相色谱测定枸杞中速灭威、克百威、抗蚜威的残留量.[方法]用乙腈提取,C18基质固相分散净化,甲醇-二氯甲烷(体积比1∶1)洗脱,Agilent TC-C18色谱柱,流动相为甲醇-水梯度洗脱,流速1.0 mL/min,柱温30℃,进样量20μL.[结果]速灭威和抗蚜威质量浓度1.0～100 mg/L、克百威质量浓度0.20～20 mg/L时,线性关系良好;添加水平为10～ 60 μg时,速灭威、克百威、抗蚜威的加标回收率分别为95.5％、92.4％、96.3％,RSD分别为2.34％、2.28％、3.46％.[结论]该方法准确、快速、简便,符合农药残留分析要求.

根据《农业行业标准》中的相应方法提取枸杞中的甜菜碱，通过单因素试验优化其主要工艺条件，如料液比、提取时间、络合剂加入量、络合时间等。结果表明，甜菜碱提取的最佳工艺条件为：料液比1 g ∶60 mL，提取时间2 h，提取液与络合剂的比为1∶5，络合时间2 h，在此条件下，3种不同地区枸杞中的甜菜碱含量由大到小排序为：甘肃枸杞（9．26％）＞青海枸杞（8．73％）＞宁夏中宁枸杞（8．71％）。

In this study,the microwave assisted extraction was used to extract polysaccharide from Lycium. The effect of four factors including the microwave power,extraction temperature,extraction time and extraction times were considered by orthogonal test.Results show that the optimum conditions are performed at 80℃with 2 times (each for 40 min) under the 700 W microwave power and the microwave extraction method is simply and effective.

In this study,the microwave extraction was used to extract pigment from Lycium,considering the effect of the four factors such as extraction temperature,extraction time,the ratio of solid to liquid,extraction times by orthogonal test.As a result,the optimum conditions was performed at 45℃with 2 times(each for 20 min) by the 1∶30 (g/mL) 80%ethanol solvent.The extraction rate was up to 17.14%.The microwave extraction method was simply and effective.

Four different methods such as dipping,leaf-dipping,leaf added and feeding were adopted respectively to test the different bioactivities of contacting,anti-feeding,stomach poison and inhibition of growth and development.The results showed that ethanol extracts of Acontium flavum Hand.-Mazz.exhibited obvious contacting,anti-feeding and stomach poison activity against Plutella xylostella similarly,but the growth inhibition activities was relatively weak.Furthermore,ethanol extracts from different parts of A.flavum Hand.-Mazz.such as root,pod,stem,seed and leaf showed the different bioactivities against P.xylostella.In the five parts,the extracts of root,pod and stem displayed stronger activities than the others.Thus,A.flavum Hand.-Mazz.could provided a plant resource for biopesticides.

The insecticidal activities against Plutella xylostella of ethanol extracts and alkaloid from wild and cultivated Aconi- tum flavum Hand. & Mazz were determined by dipping. The results showed that 72 hours after the application the adjusted mortality of the ethanol extracts against Plutella xylostella from wild and cultivated Aconitum flavum Hand. & Mazz. were 86.67% and 90.00%(30.0 mg / mL), respectively. The LC50 were 13.14 mg / mL and 12.37 mg / mL, respectively. The insecticidal activities of alkaloid against Plutella xylostella from wild and cultivated Aconitum flavum Hand. & Mazz. were as follows: the adjusted mortality were 90.00%(20.0 mg / mL) 72 hours after the application, and the LC50 were 6.535 mg / mL and 6.576 mg / mL, respectively. It is indicated that the insecticidal activities of wild Aconitum flavum Hand. & Mazz. were similar to that of cultivated Aconitum flavum Hand. & Mazz.. The result could provide a certain basis for effectively protecting wild plant resources.

[Aims] The toxicities of mixture of total alkaloids from Acontium flavum Hand.-Mazz. and lambda-cyhalothrin against Plutella xylostella L. were studied. [Methods] The effect of co-toxicity was evaluated by the methods of Bliss, three coordinates and Sun, respectively. Furthermore, the best ratio of the two alkaloids was optimized. [Results] The results showed that the mixtures of total alkaloid from A. flavum and lambda-cyhalothrin had obvious synergism, and the co-toxicity coefficient(CTC) was 173.28 under the proportion of 4∶1. [Conclusions] The insecticidal activity of the mixture was tested against P. xylostella, compared with the signal medicament of alkaloid from A. flavum with the LC 50 of 5.64×103mg/L and lambda-cyhalothrin of 13.35×103mg/L, the mixture exhibited more toxicity to P. xylostella with the LC 50 of 1.10×103mg/L.

采用点滴法测定了野生与人工种植伏毛铁棒锤的乙醇提取物及生物碱对枸杞蚜虫的杀虫活性.结果表明:野生与人工种植的伏毛铁棒锤乙醇提取物对枸杞蚜虫的杀虫活性72 h校正死亡率分别91.11％、93.33％,LC50值分别为9.923、9.738 g/L;野生与人工种植的伏毛铁棒锤生物碱对枸杞蚜虫的触杀活性72 h校正死亡率分别为96.67％、97.78％,LC50值分别为:2.204、2.220 g/L,野生与人工种植伏毛铁棒锤对枸杞蚜虫的杀虫活性相近.

采用点滴法测定了野生与人工种植伏毛铁棒锤的乙醇提取物及生物碱对枸杞蚜虫的杀虫活性。结果表明:野生与人工种植的伏毛铁棒锤乙醇提取物对枸杞蚜虫的杀虫活性72 h校正死亡率分别91.11%、93.33%,LC50值分别为9.923、9.738 g/L;野生与人工种植的伏毛铁棒锤生物碱对枸杞蚜虫的触杀活性72 h校正死亡率分别为96.67%、97.78%,LC50值分别为:2.204、2.220 g/L,野生与人工种植伏毛铁棒锤对枸杞蚜虫的杀虫活性相近。

The method for the determination of bifenthrin in Chinese wolfberry in Ningxia was developed by gas chromatography.The samples was extracted with acetonitrile,purified by the CARB/NH2 SPE column,and eluted with acetone-methylene chloride.Then the eluate was cleaned up by passing through a Florisil cartridge,which was washed with n-hexane-methylene chloride,and the analyte was eluted with ethyl acetate,and solubilized with n-hexane,finally analyzed with GC-ECD after isolated by DB-1701 capillary column.The amount of residue of bifenthrin in Chinese wolfberry was 0.002 2 μg/g and the RSD was 3.55%.The recovery was 92.47% and the RSD was 1.70%.The method was suitable for the detection of the residue of bifenthrin in Chinese wolfberry,which was simple,rapid,sensitive and accurate.The results could be useful for the quality control of Chinese wolfberry.

The liposoluble constituents were extracted by cold-soak extraction,and GC-MS was used to analyze their chemical composition,30 compounds were extracted from the foot of Euphorbia sieboldiana,28 compounds were identified,amounting for 98.42% of total constituents.Most of them are the unsaturated fatty acid-ester content up to 71.09%,the following is volatile oil 14.84%,acids 2.2%,diolefine 0.44%.The consequences indicated that the major liposoluble constituents were α-methyl linolenate(21.56%),palmitoleic acid ethyl ester(15.20%),ethyl 9,12-Octadecadienoic acid ethyl ester(14.00%),cubeb oil enol(7.84%) and Germacrene D-4-enol(7.07%).

Objective To establish a method for the determination of glycyrrhizic acid and cAMP in Guilong kechuanning capsules(traditional Chinese medicines).Methods Analyses were carried out on Agilent TC-C18(4.6 mm×150 mm,5 μm)column.The mobile phase was methanol(A)-0.01 mol · L-1 KH2PO4(B)with gradient elution[0-12 min,10%(φ)A;12-30 min,70%(φ)A],the flow rate was 1.0 mL · min-1,the detection wavelength was set at 250 nm,the column temperature was 30 ℃.Results The linear calibration curve was obtained in the concentration range of 2.0-200.0 mg · L-1 for cAMP and the glycyrrhizic acid.The mean recoveries of cAMP and glycyrrhizic acid were 95.9%(RSD=2.9%,n=3)and 92.7%(RSD=3.1%,n=3),respectively.Conclusions The method can be used to control the quality of Guilong kechuanning capsules.