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建立了能同时检测谷类食物中杀鼠酮、异杀鼠酮、敌鼠、氯敌鼠的高效液相色谱分析法。在磷酸盐缓冲溶液(pH=5.5)中用乙醇一乙酸乙酯(体积比5:95)作萃取剂,通过正交试验优化提取条件,在ZORBAX SB C18柱(250mm×4.6mmi.d.,5μm)上以磷酸盐缓冲液(pH=6.3)、乙腈、甲醇组成的流动相进行梯度洗脱分离,紫外检测。结果表明,杀鼠酮、异杀鼠酮在0.25~50.0mg/L,敌鼠、氯敌鼠在0.50~100mg/L均具有良好的线性,其相关系数均大于0.9993;杀鼠酮和异杀鼠酮的检出限均为0.1mg/L,敌鼠和氯敌鼠的检出限均为0.2mg/L;4种鼠药的回收率为80%~95%;RSD均小于8.0%。该法适用于谷类食物中茚满二酮类鼠药残留的检测。 相似文献
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建立了中毒应急检测样品生物体液内痕量敌鼠和氯敌鼠的高效液相色谱-离子阱质谱定性定量检测方法。全血样品由甲醇/乙腈(50/50, v/v)沉淀蛋白后再经Oasis HLB固相萃取小柱净化富集,尿液样品直接经同类小柱净化富集。采用Extend C18柱分离,以乙酸铵-乙酸(0.02 mol/L, pH 5.5)缓冲溶液和甲醇(15/85, v/v)溶液为流动相,使用电喷雾电离负离子多反应监测模式检测敌鼠和氯敌鼠。对全血样品,敌鼠和氯敌鼠分别在1.0~200.0 μg/L和0.5~100.0 μg/L范围内呈良好的线性关系,回收率分别在90.1%~92.2%和87.6%~93.4%范围内,日内相对标准偏差(RSD)分别小于6.8%和7.1%,日间RSD分别小于9.9%和10.9%,定量限分别为1.0 μg/L和0.5 μg/L。对尿液样品,敌鼠和氯敌鼠分别在0.2~ 40.0 μg/L和0.1~20.0 μg/L范围内呈良好的线性关系,回收率分别在90.1%~94.5%和90.0%~ 98.0%范围内,日内RSD分别小于6.1%和7.3%,日间RSD分别小于8.9%和11.2%,定量限分别为0.2 μg/L和0.1 μg/L。本方法简便、灵敏,能满足敌鼠和氯敌鼠中毒病人的临床快速诊断要求。 相似文献
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肝中茚满二酮类杀鼠剂固相萃取-紫外导数光谱检测法 总被引:2,自引:0,他引:2
报道了肝中敌鼠,氯敌鼠,杀鼠酮三种茚满二酮类杀鼠剂的题示检测方法。肝匀浆先用乙腈或二甲基甲酰胺浸提,浸提液用6%高氯酸溶液或0.1mol/L氢氧化钠溶液稀释,然后加入GDX101大孔树脂萃取,肝中杀鼠剂萃取率约80%,检出限为1μg/g以下 相似文献
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导数分光光度法测定毒饵中的敌鼠钠 总被引:2,自引:0,他引:2
用紫外二阶导数分光光度法测定毒饵中敌鼠钠含量。当样品中含有0.4g·L-1、2g·L-1敌鼠钠时平均回收率为96.8%。标准曲线范围为1~5mg·L-1,相关系数为0.9998,相对标准偏差为0.6%~2.2%,检出限为0.15mg·L-1。 相似文献
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《理化检验(化学分册)》2010,(6)
土壤样品经氢氧化钠提取后,其中不易溶于水的五氯酚以易溶于水的五氯酚钠形式被提取出来,采用紫外分光光度法测定土壤中五氯酚的含量。考察了介质的pH值、固液比及提取时间对测定的影响。在优化的试验条件下,五氯酚钠的质量浓度在40 mg.L-1以内与其吸光度呈线性关系,检出限(3S/N)为0.023 mg.L-1。用此方法测定土壤中五氯酚含量,加标回收率为94.4%~104.7%。 相似文献
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高效液相色谱法测定除草剂中二氯喹啉酸的含量 总被引:1,自引:0,他引:1
本文报道酸抑制反相色谱法测定除草剂中二氯喹啉酸的含量,该法采用PC8-10/S2504(4.0mmi.d.×250mm,10μm)柱,以甲醇-0.1%醋酸为流动相,紫外检测波长为240nm,0.08AUFS,以2,4-二硝基氯苯为内标物,样品用四氢呋喃提取,该法灵敏度及回收率高,结果定量准确,操作简便可靠。 相似文献
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分别采用紫外分光光度法测定二氢乳清酸(DHO)的减少量、PDAB显色法测定N-氨甲酰-天冬氨酸(CA-asp)的生成量来测定二氢乳清酸酶酶活,并对两种方法进行了比较。结果表明紫外分光光度法和PDAB显色法均有良好的回收率,分别为99.4%~101.2%、98.0%~101.3%。但由于PDAB显色法的检测范围为0.05~1.00g/L,较紫外法的检测范围0.05~0.30g/L更为宽泛,仪器要求低,便于实际操作。因此,采用PDAB显色法测定二氢乳清酸酶酶活较为方便。 相似文献
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用溶胶-凝胶法以磷钼酸(MPA)的镍盐溶液水解钛酸四丁酯制备了NiPMo/TiO2催化剂.使用ICP、 XRD、 TG-DTA、 IR、 TPD-MS和微反应技术研究了催化剂的化学组成、热稳定性、化学吸附性质和催化反应性能.杂多钼酸盐与TiO2通过O2-在TiO2表面发生了键合.在623 K下,杂多阴离子仍保持原有的Keggin结构.CO2在Lewis酸位Ni(Ⅱ)和Lewis碱位Ni-O-Mo的桥氧协同作用下生成CO2卧式吸附态Ni(Ⅱ)←O-(CO)←(O--Ni).丙烯有多种吸附态在催化剂上吸附.在563 K、 1 MPa和空速1500 h-1的反应条件下,丙烯的摩尔转化率为3.2%,产物MAA选择性为95%. 相似文献
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Different approaches for the synthesis of 1-benzyloxypyrazin-2(1H)-one derivatives from simple amino acids have been investigated. A library of 33 precursors for the preparation of N-hydroxy pyrazinones was obtained in moderate to good yields. 相似文献
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Toward new camptothecins. Part 6: Synthesis of crucial ketones and their use in Friedländer reaction
Laurent Gavara Thomas Boisse Jean-Pierre Hénichart Adam Daïch Philippe Gautret 《Tetrahedron》2010,66(38):7544-5571
In the context of the preparation of camptothecin and luotonin A analogs, the synthesis of some key keto-precursors and their use in Friedländer condensation are described. This paper also focuses on the stability of these keto intermediates and emphasizes the major differences between indolizinones and pyrroloquinazolinones series. Noteworthy is also the report of some original structures isolated as by-products of some experiments. 相似文献
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The Langevin paramagnetic theory can’t describe the relation between magnetization of ferrofluids and applied magnetic field. The structuralization of ferrofluids, which is considered the main influence factor of the magnetization, is regarded. The part of magnetization works is deposited when the structure is forming. This action influences the magnetization of ferrofluids directly or indirectly. On the base of the “compressing” model, the Langevin function that usually describes the magnetization of ferrofluid is modified, and a well-fitted curve is obtained. An equation of the relation between the equivalent volume fraction after being “compressed” and the intensity of magnetic field is discovered, which approximately describes the process of magnetization. The relation between the approximate initial susceptibility and the volume fraction can be obtained from modified formula. 相似文献
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Rebecca J. Burton Mandy L. CrowtherNeal J. Fazakerley Shaun M. FilleryBarry M. Hayter Jason G. KettleCaroline A. McMillan Paula PerkinsPeter Robins Peter M. SmithEmma J. Williams Gail L. Wrigley 《Tetrahedron letters》2013
The highly regioselective Buchwald–Hartwig amination at C-2 of the cheap and readily accessible reagent, 2,4-dichloropyridine with a range of anilines and heterocyclic amines is described. This new methodology is robust and provides a facile access to 4-chloro-N-phenylpyridin-2-amines on 0.25 mol scale. These intermediates undergo a further Buchwald–Hartwig amination at higher temperature to enable rapid exploration of the chemical space at C-4 and to provide a library of 2,4-bisaminopyridines. 相似文献
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KMnO4-mediated oxidative CN bond cleavage of tertiary amines producing secondary amine was introduced, which was trapped by electrophiles (acyl chloride and sulfonyl chloride) to form amides and sulfonamides. The reaction could take place at mild condition, tolerating a wide range of function groups and affording products in moderate to excellent yields. 相似文献
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N. A. Nedolya 《Chemistry of Heterocyclic Compounds》2008,44(10):1165-1219
The review contains a concise historical account and information on the most significant researches undertaken by the staff
at the A. E. Favorsky Irkutsk Institute of Chemistry, Siberian Branch of the Russian Academy of Sciences on the Chemistry
of Heterocyclic Compounds.
Dedicated to Academician of the Russian Academy of Sciences B. A. Trofimov on his 70th jubilee.
Translated from Khimiya Geterotsiklicheskikh Soedinenii, No. 10, pp. 1443–1502, October, 2008. 相似文献
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Regiospecific and direct imidation of the methyl C(sp3)–H bond of thioanisoles is realized under mild and metal-free conditions with N-fluorobis(benzenesulfonyl)imide as an oxidant and nitrogen source. Proposed mechanism suggests that thionium ion intermediates and a Pummerer-type reaction are involved. The imidation has advantages such as high step-economy, excellent functionality tolerance, and regiospecificity, giving structurally diverse imidation products. 相似文献
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A general synthesis of previously unknown semicarbazone-based α-amidoalkylating reagents, 4-(tosylmethyl)semicarbazones, has been developed. The synthesis involved three-component condensation of semicarbazones of aliphatic or aromatic aldehydes with the same or other aldehydes and p-toluenesulfinic acid. The scope and limitations of this reaction were investigated. The compounds obtained were demonstrated to be an efficient α-(4-semicarbazono)alkylating agents. They were reacted with H- (sodium borohydride), O- (sodium methylate), S- (sodium phenylthiolate), N- (pyrrolidine, sodium succinimide), P- (trialkyl phosphites), and C-nucleophiles (sodium diethyl malonate) to give the corresponding products of the tosyl group substitution, 4-substituted semicarbazones, including analogues of nitrofurazone. Among the prepared compounds tested in vitro for antibacterial and antifungal activity, three nitrofuryl-containing semicarbazones exhibited high biological activities with minimum inhibitory concentration (MIC) values of 8–32 μg/mL. 相似文献
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A small library of new chiral bidentate hydroxyalkyl-imidazolium salts 1 is conveniently synthesized on multi-gram scale from inexpensive and commercially available chiral pool amino acids. The corresponding carbenes, generated by deprotonation of imidazolium salts 1, in combination with palladium(II) chloride were tested in the Mizoroki–Heck coupling reaction. The most significant results in terms of yields and reactivities were achieved with low catalyst loading. The catalytic activities of these imidazolium salts were also investigated in the asymmetric addition of diethylzinc to benzaldehyde. The use of MgO nanoparticles as an additive in conjunction with these ligands played a crucial role in increasing the efficiency of these reactions. 相似文献