共查询到20条相似文献,搜索用时 68 毫秒
1.
建立了血清中苯巴比妥、苯妥英钠和卡马西平的胶束电动毛细管色谱(MEKC)分析法。方法以巴比妥钠为内标物,10 mmol/L磷酸氢二钠溶液-30 mmol/L十二烷基硫酸钠(胶束相)-15%甲醇为缓冲液(pH=8.50),恒定电压18 kV,检测波长210 nm。本法测定苯巴比妥和苯妥英钠两种药物的线性范围为2.5~80μg/mL(r≥0.9990),检出限为0.5μg/mL;测定卡马西平的线性范围为1~32μg/mL(r=0.9999),检出限为1.0μg/mL。方法快速、简便、结果准确,适合于临床应用。 相似文献
2.
测定了1562名儿童(其中包括153名易疲劳儿童)血清中Zn、Fe、Cu、Ca、Mn和Pb的含量。研究发现,易疲劳儿血清Ca含量(84.4±12.5μg/mL)显著低于对照组儿童(88.5 4±13.4μg/mL),P<0.05;Fe含量(1.094±0.22μg/mL)显著高于对照组儿童(1.07 4±0.22μg/mL),P<0.05;Mn含量(0.040 4±0.035μg/mL)非常显著高于对照组儿童(0.035 4±0.013μg/mL),P<0.001。 相似文献
3.
儿童神经过敏与血清中6种无机元素含量相关性研究 总被引:2,自引:0,他引:2
王美绮 《广东微量元素科学》2002,9(8):33-35
测定了1261名儿童(其中包括73名神经过敏儿童)血清中Zn、Fe、Cu、Ca、Mn和Pb的含量。研究发现,神经过敏患儿血清Zn含量(0.95±0.20μg/mL)显著低于对照组儿童(0.97±0.23μg/mL),P<0.05;Mn含量(0.03±0.01μg/mL)非常显著低于对照组儿童(0.04±0.02μg/mL),P<0.01。 相似文献
4.
建立了高效液相色谱法(HPLC)同时测定24种花中绿原酸、金丝桃苷、槲皮素、木犀草素和异鼠李素含量的方法。采用C18柱(250 mm×4.6 mm,5μm),流动相为甲醇-0.2%冰乙酸溶液梯度洗脱,检测波长350 nm,柱温35℃,流速0.8 mL/min。绿原酸、金丝桃苷、槲皮素、木犀草素和异鼠李素分别在0.0208~104.00μg/mL(r=0.99993),0.017~85.00μg/mL(r=0.99998),0.0172~86.00μg/mL(r=0.99997),0.0304~152.00μg/mL(r=0.99997),0.0168~84.00μg/mL(r=0.99986)范围内与峰面积呈良好的线性关系,平均加标回收率(n=9)92.26%~99.09%,仪器精密度(n=6)RSD均小于3.1%,方法重复性(n=6)的RSD均小于3.6%。方法可同时测定这24种花中绿原酸和黄酮类物质的含量,可作为花中活性成分定量分析的方法。 相似文献
5.
高效液相色谱法测定九味石灰华散中羟基红花黄色素A和红景天苷的含量 总被引:1,自引:0,他引:1
建立了测定中药复方制剂九味石灰华散中羟基红花黄色素A和红景天苷含量的高效液相色谱方法.采用Kromasil C18色谱柱(5μm,250 mm×4.6 mm),以乙腈∶0.1%磷酸溶液(12∶88,V/V)为流动相,流速1.0 mL/min,羟基红花黄色素A的检测波长为403 nm,红景天苷的检测波长为275 nm.羟基红花黄色素A和红景天苷分别在0.288~180μg/mL和4.8~1 200μg/mL范围内呈良好的线性关系(r值为0.999 8~0.999 9),最低检出限分别为0.03μg/mL和0.5μg/mL(S/N=3),加标回收率分别为95.7%~97.4%和95.9%~98.6%.该方法简便、准确、重现性好,可用于九味石灰华散的质量控制. 相似文献
6.
7.
用反相高效液相色谱法追踪分析不同时间内羊血清中药物浓度的变化,以供药物代谢动力学研究.药物为丙硫咪唑砜和丙硫咪唑亚砜(简称砜和亚砜),实验条件为ODS柱,流动相甲醇:水=7:3(v/v),紫外检测波长为290nm.在3h左右测定浓度达峰值,其最高浓度分别为4.01μg/mL和11.47μg/mL,五天左右下降为2.73μg/mL和1.32μg/mL附近.最小检出量为0.4ng/mL及0.7ng/mL.线性关系良好.丙硫咪唑砜和亚砜的回归相关系数分别为0.9994和0.9991.采用内标法测定回收率,平均为 相似文献
8.
建立尿液中曲马多的顶空固相微萃取气相色谱质谱联用(HS-SPME-GC/MS)分析方法。利用响应面法对顶空固相微萃取的条件进行优化,在优化的条件下,采用SKF为内标,在选择离子模式下,选取m/z 58(曲马多)和m/z 86(SKF)为定量离子,利用GC/MS对尿液中的曲马多进行定量分析。工作曲线线性范围超过0.05~1.0μg/mL(r2=0.9962)。检测限为0.011μg/mL(S/N=3),定量限为0.038μg/mL(S/N=10),用0.1μg/mL和0.75μg/mL曲马多标准液计算回收率分别在100.20%~109.65%和98.43%~103.82%之间,RSD为5.32%和9.13%(n=5)。建立的方法适用于尿液中曲马多。 相似文献
9.
采用顶空气相色谱技术,建立了同时测定新药CBT108中12种残留溶剂的方法。优化了平衡加热时间和程序升温时间以及制样的溶剂,并通过验证确定了本方法的合理性、准确性和可行性。在优化的实验条件下,采用DB-624型毛细管柱(6%氰丙基苯基-94%二甲基聚硅氧烷为固定液,30 m×0.53 mm×3.0μm)分离、氢火焰离子化检测器检测、内标法定量的分析方案,实现了甲醇、乙醇、乙醚、丙酮、乙腈、二氯甲烷、正己烷、乙酸乙酯、四氢呋喃、庚烷、甲苯和四氯化碳共12种残留溶剂的同时分离与测定。12种溶剂在各自的范围内线性关系良好,线性相关系数(R~2)均0.997;以10倍信噪比确定方法定量限,以3倍信噪比确定方法检出限,分别为:甲醇0.024μg/mL、0.0072μg/mL;乙醇0.1μg/mL、0.012μg/mL;乙醚0.01μg/mL、0.005μg/mL;丙酮0.1μg/mL、0.008μg/mL;乙腈1.025μg/mL、0.0615μg/mL;二氯甲烷0.09μg/mL、0.06μg/mL;正己烷0.0174μg/mL、0.0145μg/mL;乙酸乙酯0.25μg/mL、0.008μg/mL;四氢呋喃0.108μg/mL、0.014μg/mL;四氯化碳0.16μg/mL、0.0004μg/mL;庚烷0.0075μg/mL、0.005μg/mL;甲苯0.0445μg/mL、0.0014μg/mL。在3个添加水平下,12种残留溶剂的加标回收率在90.96%~108.67%之间,相对标准偏差为0.1%~5.7%。结果表明,本法简单、快速、重现性好、准确性高,可用于实际药品中以上12种残留溶剂的检测,并可对其它药物中残留溶剂的检测提供参考。 相似文献
10.
建立了一种同时分离测定人体尿液中4种蝶呤类化合物(新蝶呤、异黄蝶呤、蝶呤和生物蝶呤)的高效液相色谱法。采用SHIMADZU Shim-pack:Vp-ODS(250 mm×4.6 mm×5μm)色谱柱结合荧光检测器,在流动相为甲醇-水(10+90),流速1.0mL/min,荧光检测波长Ex390 nm,Em450 nm,柱温为室温的色谱条件下,4种蝶呤类化合物分离效果良好。尿液经0.45μm的一次性滤膜过滤,取10μL滤液直接进样测定。结果表明,各组分的线性范围为:新蝶呤0.05~1.20μg/mL,异黄蝶呤0.05~0.80μg/mL,蝶呤0.05~1.00μg/mL,生物蝶呤0.05~1.00μg/mL。4种组分的检测限均为0.01μg/mL。该方法可应用于临床癌症病人和健康人尿样中4种蝶呤类化合物的检测。 相似文献
11.
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
12.
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
13.
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
14.
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
15.
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
16.
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
17.
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
18.
19.
《Tetrahedron》2014,70(21):3377-3384
The Rh(II)-catalyzed reaction of 2-carbonyl-substituted 2H-azirines with ethyl 2-cyano-2-diazoacetate or 2-diazo-3,3,3-trifluoropropionate provides an easy access to 2H-1,3-oxazines and 1H-pyrrol-3(2H)-ones. These compounds can be selectively prepared from the same starting material using temperature as the only varied parameter. The 2-azabuta-1,3-diene intermediate, a common precursor for both heterocyclic products, isomerizes into 2H-1,3-oxazine under kinetic control, while 1H-pyrrol-3(2H)-one is the sole product of the reaction at elevated temperatures. According to DFT-calculations a one-atom oxazine ring contraction involving ring-opening to a 2-azabuta-1,3-diene intermediate, followed by a 1,5- and 1,2-prototropic shift leads to the consecutive formation of imidoylketene and azomethine ylide, which then further undergo cyclization to the pyrrole derivative. 相似文献
20.
袁都奇 《化学物理学报(中文版)》2001,14(3):381-384
把有限时间热力学理论用于化学过程的研究,将会得到一系列新的结论,开展这方面的研究是很有意义的.文献[1]以燃料电池为例,在同时考虑化学反应及传热不可逆性的情况下,研究了燃料电池的性能界限,文献[2]指出了文献[1]计算化学反应及传热不可逆性而引起系统与有关环境的总熵产生率的错误以及由此而导致的结论所存在的问题,并进行了富有启发性的分析与讨论.但文献[2]对于系统与有关环境的总熵产生率的计算也是不正确的,由此得到的其它结论自然不能成立.本文将就此情况下系统与有关环境的总熵产生率的计算再次进行讨论,并给出电池功率和效率的有限时间热力学性能界限. 相似文献