(三唑基-~(14)C-)粉锈宁的标记合成

本文报道了(三唑基-14C)-粉锈宁的制备。由14C-甲酸和重碳酸氨基胍形成(5-14C)-3-氨基-1,2,4-三唑,再经重氮化脱氨得到(5-14C)-1,2,4-三唑,最后再与对氯酚和二氯片呐酮反应得到(三唑基-14C)-粉锈宁。放化收率为26％(从甲酸-14C计),放化纯度大于95％。     

油菜对~(35)SO_4~(2-)吸收和种子中硫代萄萄糖苷的累积

砂培油菜苗能迅速从培养液中吸收~(35)SO_4~(2-),并迅速结合到硫代葡萄糖苷、氨基酸和蛋白质中。标记后,70％甲醇抽提的~(35)S申硫苷-~(35)S的百分含量随时间有规律地下降,而氨基酸中的~(35)S相应地上升。结合成分中~(35)S的相对含量在标记5天后保持恒定。开花后两周,豆荚和籽粒中硫苷-~(35)S的相对含量随时间线性增加,至开花后8周,种子中70％甲醇抽提成分的~(35)S均为硫苷-~(35)S。豆荚和籽粒中,硫苷-~(35)S与干物质含量均随时间线性增加。     

除草剂虎威的标记合成

5-( 2-氯-4-三氧甲基 )苯氧基 )- N-(甲基磺酰基 ) - 2-硝基苯甲酰胺 (虎威 )的14 C标记合成经 6步完成。其放化收率为 1 8 1 5 % (以14 C 以苯甲酸计 ) ,放化纯度经薄板检测大于 99%。     

氨甲喋呤(MTX)的直接碘标记方法研究

本文报道了~125I(~131I)抗肿瘤药物氨甲喋呤的制备方法,用直接碘化法——NBS、ChT、Iodogen进行标记,并对这几种方法进行了比较。结果表明,NBS法最好,标记率达90—99％。经Sephadex G-75柱凝胶过滤后得到纯产品,放化纯度为95.4％。所制得的标记产品适用于示踪研究。     

高比活度碳-14标记氟噻草胺的合成与分析

为开展除草剂氟噻草胺在我国的登记代谢试验,本研究以4-氟[U-¹⁴C]苯胺为同位素原料,经还原胺化、缩合、取代、水解和醚化五步放化反应获得N-(4-氟[U-¹⁴C]苯基)-N-异丙基-2-((5-(三氟甲基)-1,3,4-噻二唑-2-基)氧基)乙酰胺(2,总活度201.65 MBq;比活度2 049.80 MBq·mmol^-1;化学纯度和放化纯度均大于98%,总放化收率39%);以[¹⁴C]硫氰酸钠为同位素原料,经加成、水解、环化、重氮化和醚化五步放化反应获得N-(4-氟苯基)-N-异丙基-2-((5-(三氟甲基)-1,3,4-[2-¹⁴C]噻二唑-2-基)氧基)乙酰胺(3,总活度287.86 MBq;比活度2 042.40 MBq·mmol^-1;化学纯度和放化纯度均大于98%,总放化收率14%)。两种标记物的结构经核磁共振氢谱(¹H NMR)和质谱(MS)分析确认,质量指标经高效液相色谱(HPLC-PDA)、放射性薄层成像分析(TLC-IIA)、在线放射性高效液相色谱(HPLC-FSA)和液体闪烁法(LSC)测定,均可作为放射性示踪剂。本研究结果为氟噻草胺的同位素示踪研究(包括该除草剂在我国的登记代谢试验)奠定了物质基础。     

(~(14)C-三唑基)-多效唑的合成

用相转移催化法标记合成了植物生长延缓剂1-对氯苯基-2-[(5-(14)~C)-1,2,4-三唑-1-基]4,4-二甲戊-3-醇((14)~C-多效唑)。其步骤包括在相转移催化剂PEG800的存在下,(5-(14)~C)-1,2,4-三唑与一氯片呐酮在乙酸乙酯溶液中反应,生成(5-(14)~C)-α-三唑基片呐酮,后者在苯溶液中再与对氯氯苄反应,生成(14)~C-三唑酮,最后在甲醇溶液中用硼氢化钠还原得到(14)~C-多效唑。其总放化收率为20.9％(以(14)~C-三唑计),放化纯度大于99％。     

西维因和1-萘酚的结合残留在土壤中的释放、矿化及植物吸收

<正> 材料和方法药品:示踪原子标记在1-萘酚位置的~(14)C-西维因(放射性强度3.11毫居里/克),1-(1-~(14)C)萘酚(放射性强度20.1毫居里/毫摩尔)。土壤:一种粘土;其特性:有机碳1.5％,砂12％,淤泥15％,粘土73％,pH值7.3。结合残留土壤的制备:含有60％水份的潮湿粘土(风干重50克),分别用~(14)C-西维因或~(14)C-1-萘酚处理,使得土壤中的浓度为10ppm,这些土壤放在一个连续流动的系统     

NaCl+Na_2SO_4胁迫对甜菜根际土壤微生物数量及酶活性的影响

为了探究NaCl+Na_2SO_4胁迫下甜菜根际环境的变化,选用KWS0143和Beta464 2个品种为材料,在盆栽条件下,将Na Cl和Na_2SO_4以摩尔比2∶1混合,按Na占土壤质量百分比为0、0.2%、0.3%和0.4%(S0、S2、S3和S4)设置4个处理,研究不同程度盐胁迫对甜菜根际土壤微生物数量和土壤酶活性的影响。结果表明,胁迫处理下根际土壤真菌、细菌和放线菌数量差异显著,细菌(18.19×10~5~176.23×10~5CFU·g~(-1))放线菌(7.08×10~5~35.18×10~5CFU·g~(-1))真菌(0.18×10~5~0.98×10~5CFU·g~(-1))。同一取样时期,各处理之间比较,土壤脲酶、磷酸酶、过氧化氢酶活性和微生物总量均是S3最高;2个品种的根际土壤微生物数量和酶活性在取样后期差异均显著,KWS0143高于Beta464。相关分析表明,脲酶活性与细菌数量和微生物总量,过氧化氢酶活性与放线菌数量均呈显著正相关。由此可见,一定量的盐胁迫有利于提高甜菜根际土壤微生物数量及酶活性。本研究为调控盐渍土甜菜生长提供了理论依据。     

模拟干旱和盐碱胁迫对碱蓬、盐地碱蓬种子萌发的影响

为研究干旱和盐碱胁迫对碱蓬(Suaeda glauca)、盐地碱蓬(Suaeda salsa)种子萌发的影响,比较碱蓬和盐地碱蓬逆境生理特性的异同,本研究利用PEG6000、NaCl和Na_2CO_3分别模拟干旱、盐和碱胁迫,配制相同渗透势的PEG6000、NaCl、Na_2CO_3处理液,以蒸馏水处理为对照,对碱蓬、盐地碱蓬种子的萌发与胚的生长进行比较研究。结果表明:1)低渗处理(-0.46 MPa)对碱蓬、盐地碱蓬种子的萌发无显著影响;高渗处理(-1.38MPa、-1.84 MPa)抑制碱蓬、盐地碱蓬种子的萌发。2)当溶液渗透势相等时,NaCl处理下碱蓬种子的萌发率显著大于PEG、Na_2CO_3处理;而等渗PEG、NaCl、Na_2CO_3处理对盐地碱蓬种子萌发率的影响无显著差异。3)PEG、NaCl、Na_2CO_3处理组碱蓬、盐地碱蓬种子的最终萌发率与对照无显著差异。4)在幼苗形成阶段,PEG、Na_2CO_3处理对碱蓬、盐地碱蓬胚的抑制作用显著大于等渗NaCl处理。5)碱蓬、盐地碱蓬胚的生长对NaCl、Na_2CO_3胁迫的响应存在差异。-0.92 MPa NaCl处理抑制碱蓬胚的生长,却对盐地碱蓬产生促进作用;-0.46 MPa Na_2CO_3处理对碱蓬胚的抑制作用小于盐地碱蓬。综合分析表明:碱蓬、盐地碱蓬均具有很强的抗盐性。在种子萌发阶段,碱蓬种子的抗旱、抗碱能力低于盐地碱蓬;在幼苗形成阶段,碱蓬胚的抗盐性小于盐地碱蓬,但对轻度碱胁迫的抗性高于盐地碱蓬。     

无机硒肥对土壤有效氮含量及菠菜品质的影响

【目的】研究不同浓度亚硒酸钠(Na_2SeO_3)对土壤脲酶活性、铵态氮(NH_4^+-N)和硝态氮(NO_3~–-N)含量及菠菜品质的影响,综合分析Na_2SeO_3在土壤-根部-作物之间被吸收、转运、转化的可能路径,为生物强化生产富硒农产品及调控硒的安全水平提供参考。【方法】进行连续42天盆栽试验,共设置4个处理,每千克土施Na_2SeO_3 0 (对照)、1、10、30 mg,分别于定植后的14、28、42天测定菠菜叶可溶性糖、可溶性蛋白、维生素C、硝酸盐含量,并测定土壤铵态氮、硝态氮含量及土壤脲酶活性等指标。【结果】在菠菜生长期间,≤10mg/kg Na_2SeO_3处理可使土壤脲酶活性表现为先被激活后减弱至对照水平,土壤硝态氮含量也表现出相同的变化趋势,但铵态氮变化趋势正好相反;30 mg/kg Na_2SeO_3处理对土壤脲酶活性没有明显的影响,在整个培养时期与对照水平相当,土壤NH_4^+-N含量后期明显减少,转化成的NO_3~–-N含量明显增加,有利于菠菜吸收利用。同等Na_2SeO_3添加量条件下,Na_2SeO_3对三个取样时间菠菜叶的硝酸盐、维生素C (Vc)、可溶性蛋白、可溶性糖含量影响各异。1 mg/kg Na_2SeO_3处理组可使菠菜叶的硝酸盐含量明显增加,Vc含量先增后减,可溶性蛋白含量减少,可溶性糖含量没有变化;10 mg/kg处理组可使菠菜叶中的硝酸盐、可溶性糖含量表现为先增后减,Vc含量、可溶性蛋白含量均有不同程度增加;30 mg/kg处理组可使菠菜叶的硝酸盐含量先增后减,可溶性蛋白、可溶性糖含量减少,Vc含量没有变化。【结论】不同浓度亚硒酸钠对土壤有效氮及菠菜品质有不同程度的影响。富硒作物生产中无机硒肥施用量要综合考虑硒在作物体内的转化率及硒对作物品质影响的各项因素而确定。     

14C-标记氧化乐果的合成

杀虫剂氧化乐果(O,O-二甲基-S-(N-甲氨基甲酰甲基)硫赶磷酸酯)的14C标记合成经4步完成。其放化收率为27.81%(以14C-碳酸钡计),放化纯度经薄板检测大于95%。     

Synthesis of (-)-[4-3H]epigallocatechin gallate and its metabolic fate in rats after intravenous administration

Because a great deal of attention has been focused on the metabolism of (-)-epigallocatechin gallate (EGCg), quantitative analysis of this compound is required. For this purpose we developed a method of chemical synthesis of [4-(3)H]EGCg. Synthesized [4-(3)H]EGCg showed 99.5% radiochemical purity and a specific activity of 13 Ci/mmol. To clarify the excretion route of EGCg, the radioactivity levels of bile and urine were quantified after intravenous administration of [4-(3)H]EGCg to bile-duct-cannulated rats. Results showed that the radioactivity of the bile sample excreted within 48 h accounted for 77.0% of the dose, whereas only 2.0% of the dose was recovered in the urine. The excretion ratio of bile to urine was calculated to be about 97:3. These results clearly showed that bile was the major excretion route of EGCg. Time-course analysis of the radioactivity in blood was also performed to estimate the pharmacokinetic parameters following intravenous administration of [4-(3)H]EGCg. In addition, EGCg metabolites excreted in the bile within 4 h after the intravenous dose of [4-(3)H]EGCg were analyzed by HPLC. The results showed that 4',4"-di-O-methyl-EGCg was present in the conjugated form and made up about 14.7% of the administered radioactivity.     

放射性同位素示踪试验需要注意的若干问题

本文对目前国内放射性同位素示踪试验过程中有关示踪剂选择、引入量估算、示踪剂引入方法、放射性样品预处理以及放射性测量方法(尤其是液体闪烁测量)中所存在的常见问题进行了简要剖析,以期对从事放射性同位素示踪研究的人员有所助益。     

Synthesis of structured lipids containing medium-chain and omega-3 fatty acids

The ability of different lipases to incorporate omega3 fatty acids, namely, eicosapentaenoic acid (EPA, C20:5n-3), docosapentaenoic acid (DPA, C22:5n-3), and docosahexaenoic acid (DHA, C22:6n-3), into a high-laurate canola oil, known as Laurical 35, was studied. Lipases from Mucor miehei (Lipozyme-IM), Pseudomonas sp. (PS-30), and Candida rugosa (AY-30) catalyzed optimum incorporation of EPA, DPA, and DHA into Laurical 35, respectively. Other lipases used were Candida anatrctica (Novozyme-435) and Aspergillus niger (AP-12). Response surface methodology (RSM) was used to obtain a maximum incorporation of EPA, DPA, and DHA into high-laurate canola oil. The process variables studied were the amount of enzyme (2-6%), reaction temperature (35-55 degrees C), and incubation time (12-36 h). The amount of water added and mole ratio of substrates (oil to n-3 fatty acids) were kept at 2% and 1:3, respectively. The maximum incorporation of EPA (62.2%) into Laurical 35 was predicted at 4.36% of enzyme load and 43.2 degrees C over 23.9 h. Under optimum conditions (5.41% enzyme; 38.7 degrees C; 33.5 h), the incorporation of DPA into high-laurate canola oil was 50.8%. The corresponding maximum incorporation of DHA (34.1%) into Laurical 35 was obtained using 5.25% enzyme, at 43.7 degrees C, over 44.7 h. Thus, the number of double bonds and the chain length of fatty acids had a marked effect on the incorporation omega3 fatty acids into Laurical 35. EPA and DHA were mainly esterified to the sn-1,3 positions of the modified oils, whereas DPA was randomly distributed over the three positions of the triacylglycerol molecules. Meanwhile, lauric acid remained esterified mainly to the sn-1 and sn-3 positions of the modified oils. Enzymatically modified Laurical 35 with EPA, DPA, or DHA had higher conjugated diene (CD) and thiobarbituric acid reactive substance (TBARS) values than their unmodified counterpart. Thus, enzymatically modified oils were more susceptible to oxidation than their unmodified counterparts, when both CD and TBARS values were considered.     

水稻高产群体的营养平衡

Sulfur transformation in 3 soils maintained in a closed incubation system and its availability to plants were investigated using carrier-free ^35S-SO4^2- and ^35S-labeled ryegrass straw.For carrier-free Na2^35SO4 treatment,78%,70%and 64% of ^35S applied were found in Ca(H2PO4)2-extractale S fraction,4%,5% and 7% in slowly soluble inorganic S,11%,15%and 18%in C-O-S,5%,7%,and 6% in C-bonded S,and 5%,7% and 6% in unidentified organic S120 days after incubation in black soil,cinnamon soil and chestnut soil,respectively.Most of 35S uptake by plants came from extractable 35SO4^2-,and little from C-O-^35S and C-bonded ^35S,In the treatment with 35S-labeled straw,51%,46%and 36% of 35S incorporated were found in Ca(H2PO4)2-extractable S fraction,7%,6% and 7% in slowly soluble inorganic S,13%,15%and 18% in C-O-S,8%,8%and 6% in C-bonded S,and 18%,25%and 35% in unidentified organic S at the end of incubation in above-mentoned three soils,respectively.Higher availability of C-O-35S,C-bonded 35S and unidentified organic 35S from 35S-labeled straw was observed in 35S-labeled straw treatment compared to carrier-free Na2^35SO4 treatment.     

Simple method for estimating 14C in formic acid solutions using liquid scintillation counting

Abstract

The feasibility of using a simple radiochemical method to determine the extent of formylation resulting from interaction of formic acid solutions with soil constituents was investigated. The interaction between formic acid‐^l4C solvents and starch was used as a model reaction. Radioassay of 1 cm³ formic acid solution by liquid scintillation counting in 10 cm³ of the scintillator‐solubilizer Insta‐gel was found to be suitable. The method is simple to use and sample preparation is easy.