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1.
吐温80-盐-水体系的液-固萃取光度法测定痕量钴   总被引:19,自引:4,他引:15  
研究了Co(Ⅱ)-PAR在吐温80-硫酸铵体系中的最佳萃取条件,建立了生物样品中测定痕量钴的非有机溶剂液-固萃取光度法。在pH7.0~10.5的NH3.H2O-NH4Cl缓冲溶液中,1金属配合物Co(Ⅱ)-PAR可被吐温80固相富集,最大吸收波长为515nm,钴含量在0~5.0ug/mL范围内服从比尔定律,可用于头发、茶叶和维生素B12针剂中痕量钴的测定。  相似文献   

2.
用HPLC/ECD法测定血小板5-HT,运用 WatersμBondapak C柱,3,4二羟基苄胺(DH-BA)作内标,以 0.07 mol/L乙酸钠缓冲液+乙腈为流动相(20+1),每1L缓冲液含 0.05 mol/L柠檬酸、2.5 mmol/L庚烷磺酸钠、0.1mmol/L Na_2EDTA,流速0.8 mL/min。DHBA和 5-HT的保留时间分别为5.4和11.5 min,线性范围为0.025~1mg/L(r= 0.9997)。5-HT日内 RSD低于1.87%,日间RSD低于8.54%,方法回收率为100.4%±2.3%。提示本方法快速简便,灵敏准确,适用于临床基础研究。  相似文献   

3.
报道了两种9-冠-3衍生物的合成,并以合成的化合物作载体研制了对锂离子响应的PVC膜电极。以乙基-9-冠-3为载体的锂离子电极的能斯特响应为10×10-1~52×10-5mol/L,斜率为(574±03)mV/p[Li](25℃),检测下限为24×10-5mol/L。电极具有良好的稳定性和重现性,用于实际样品测定,结果满意  相似文献   

4.
研究了Os(Ⅱ)和4,4’二(二乙氨基)苯硫酮与Pt(Ⅱ)共显色所衍生的配合物,于NucleosilC_8柱上,用含3×10 ̄(-3)mol/LDL-樟脑-10-磺酸和0.02mol/LHAc-NaAc(pH3.5)的乙腈-丙酮-水(72:5:23,V/V)作流动相(1.0mL/min)分离并检测。线性范围为0.2~4.0μg/mLPt;检测限为1.0ngPt。此方法已应用于抗癌药物顺铂和卡铂的分析。  相似文献   

5.
铂—钯共显色衍生络合物的高效液相色谱研究   总被引:4,自引:3,他引:1  
张孝松  屈建 《分析化学》1993,21(12):1365-1369
研究了Pd(Ⅱ)和4,4'-二(二乙氨基)苯硫酮(BDPTK)共显色所生成的Pt(Ⅱ)络合物,于Nucleosil C8柱上,用含3×10^-3mol/L CSA和0.02mol/L HAc-NaAc(pH3.5)的乙腈-丙酮-水(72:5:23,V/V)作流动相(1.0ml/min)分离并检测。Pt的校正曲线的线性范围为0.2~3.0μg/ml,Pt检测限为0.7ng。此方法已应用于抗癌药物顺铂  相似文献   

6.
阿斯美胶囊中四种组分的高效液相色谱分析   总被引:2,自引:0,他引:2  
建立了反相高效液相色谱法测定阿斯美胶囊中氨茶碱、盐酸甲氧非那明、马来酸氯苯那敏及那可汀四种组分的含量。色谱柱为SpherisorbC8,5μm,200cm×40mmID,流动相为体积分数05%的三乙胺溶液(磷酸调节pH55)+乙腈+甲醇(550+368+82),检测波长为264nm,线性范围分别为:氨茶碱3125~250mg/L,γ=09996,盐酸甲氧非那明15625~1250mg/L,γ=10000,马来酸氯苯那敏25~200mg/L,γ=09999,那可汀875~700mg/L,γ=09999;回收率(n=3)分别为1012%,1008%,999%,995%;精密度:日内平均RSD(n=6)分别为07%,04%,04%,06%;日间平均RSD(n=3)分别为10%,10%,11%,12%。  相似文献   

7.
荧光分析法测定痕量丁二酮   总被引:5,自引:0,他引:5  
本文报道了邻苯二胺与丁二酮在1mol/LH2SO4介质中反应生成2,3-二甲基喹喔啉。该化合物具有较强的荧光(λx/λem=340nm/490nm)其荧光量子产率ΦF=0.101。丁二酮浓度在4.0×10^-7~5.2×10^-5mol/L范围内与转化成产物的相对荧光强度呈线性关系,相对标准偏差为1%,检出限为1.3×10^-7mol/L,考察了30种物质表明,该法选择性好,用于实际啤酒样品中丁二  相似文献   

8.
乳酸环丙沙星单扫描示波极谱法研究   总被引:3,自引:0,他引:3  
研究了乳酸环丙沙星的极谱伏安行为,在pH=8.3的0.02mol/L,NH4Cl-NH3.H2O底液中,乳酸环丙沙星能产生1个灵敏的还原峰,峰电位为-1.61V,其导数峰高与浓度在3.9×10^-8~1.8×10^-6mol/L和1.8×10^6~1.1×10^-5mol/L范围内呈现良好的线性关系,相关系数r=0.9997,检测下限为2.5×10^-8mol/L,用于乳酸环丙沙星注射液的测定,相  相似文献   

9.
1,2,4-三唑并[3,2-d][1,5]-苯并氧氮杂(艹/卓)化合物的合成   总被引:1,自引:1,他引:0  
苯并二氢吡喃-4-酮的芳腙(1)衍生的偶氮基碳正离子(3)与腈发生1,3-偶极环加成反应,加成产物(4)通过「1,2」-迁移扩环重反应,形成新颖的三环系杂环化合物1,2,4-三唑并「3,2-d」「1,5」-苯并氧氮杂Zhuo化合物5a-5k。  相似文献   

10.
于pH10.0~11.0的NH3-NH4Cl缓冲介质中,在TritonX-100存在下,铊(Ⅲ)与2-羟基-3-羧基-5-磺酸基苯基重氮氨基偶氮苯(HCS-DAA)形成组成比为1∶3的红色配合物,其最大吸收波长和对比度分别为510nm和80nm,表观摩尔吸光系数为1.52×105L·mol-1·cm-1,线性范围为0~0.70mg/L,室温下显色反应立即完成,配合物至少稳定2h。方法用于水样、烟叶和煤灰中痕量铊的分析,回收率为90.0%~101.4%,5次测定的相对标准偏差不大于4.6%。  相似文献   

11.
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   

12.
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   

13.
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   

14.
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   

15.
16.
A new and simple synthesis of novel N-protected methyl 5-substituted-4-hydroxypyrrole-3-carboxylates, which exist in equilibrium with their 4-oxo tautomers, has been developed in two steps starting from N-protected α-amino acids. The key intermediates are enaminones, which can also be isolated, characterized, and used for the construction of other functionalized heterocycles, before they spontaneously decompose to pyrrole products. 4-Hydroxypyrroles are prone to partial aerial oxidation but can be efficiently alkylated or reduced to stable polysubstituted pyrrolidine derivatives.  相似文献   

17.
The chemoselectivity in the intramolecular CH insertion of various diazosulfonamides has been experimentally studied. The results reveal that the aliphatic 1,4-, 1,5-, or 1,6-C(sp3)?H insertions of diazosulfonamides are not accessible, while the aromatic 1,5-C(sp2)?H insertion can be realized specifically by adjusting the diazo-adjacent group. In addition, the general chemoselectivities in the intramolecular CH insertions of diazosulfonyl compounds are summarized. Generally, diazosulfones undergo both aromatic 1,5-C(sp2)?H and aliphatic 1,5- and 1,6-C(sp3)?H insertions, while diazosulfonates undergo aliphatic 1,5- and 1,6-C(sp3)?H insertions. However, diazosulfonamides only undergo aromatic 1,5-C(sp2)?H insertion.  相似文献   

18.
Quercetin, the polyphenolic compound, which has the highest daily intake, is well known for its protective effects against aging diseases and has received a lot of attention for this reason. Both quercetin 3-O-β-d-glucuronide and quercetin 3′-O-β-d-glucuronide are human metabolites, which, together with their regioisomers, are required for biological as well as physical chemistry studies. We present here a novel synthetic route based on the sequential and selective protections of the hydroxyl functions of quercetin allowing selective glycosylation, followed by TEMPO-mediated oxidation to the glucuronide. This methodology enabled us to synthesize the five O-β-d-glucosides and four O-β-d-glucuronides of quercetin, including the major human metabolite, quercetin 3-O-β-d-glucuronide.  相似文献   

19.
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   

20.
An efficient approach to the synthesis of highly congested di, penta and hexacyclic pyrazoles as well as imidazole fragment containing novel heterocyclic molecule has been developed through a carbanion induced transformation of suitably functionalized 2H-pyran-2-ones, benzo[h]chromene and thiochromeno[4,3-b]pyrans. Due to the presence of fluorescence, we report their prime application metal sensor as off/on switching in ferric ions.  相似文献   

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