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建立了化妆品中西咪替丁及雷尼替丁的高效液相色谱-四极杆/飞行时间高分辨质谱检测方法,并对其质谱裂解规律进行研究。待测样品经甲醇超声提取,过滤膜后经Zorbax SB-Aq色谱柱(3.0 mm×100 mm,1.8μm)分离,用乙腈-含0.1%甲酸的水溶液梯度洗脱后,在双喷雾电喷雾离子源正离子模式下检测,数据采集使用一级母离子全扫描和目标二级离子扫描。在不同的化妆品基质中,西咪替丁和雷尼替丁分别在5.65~113 ng/mL和4.95~99.0 ng/mL范围内线性关系良好(r0.999),检出限分别为1.1、0.99 ng/mL,定量下限分别为5.6、5.0 ng/mL;2种待测物在低、中、高3个加标水平下的回收率为86.7%~110%,相对标准偏差(RSD)为0.90%~6.0%,方法重复性良好(RSD10%)。该方法前处理简单,灵敏度较好,线性、回收率及重复性均满足方法学要求,可用于化妆品中西咪替丁和雷尼替丁的筛查测定。  相似文献   
2.
建立以核磁共振技术测定片剂中西咪替丁含量的方法。采用Agilent DD2-500型核磁共振波谱仪,以氘代甲醇为溶剂、对苯二甲酸二甲酯为内标,测试温度25℃,弛豫时间为20 s,脉冲角为45°,采集时间为2 s,扫描次数为16次,采集核磁共振氢谱。该方法线性范围为0.1~5.0 mg/mL,相关系数r=0.999 8,测定结果的相对标准偏差为0.11%(n=6),平均加标回收率在100.03%~100.58%之间。用该方法测定不同厂家片剂中西咪替丁的含量,测定结果与药典方法相吻合。该方法简单快速、样品用量少,适用于西咪替丁的质量控制。  相似文献   
3.
Cimetidine reacting with 1,5-dichloroanthraquinone in acetone solution can produce a charge-transfer complex that shows a strong absorption peak at 343 nm. The absorption value at 343 nm increased with cimetidine concentration in the range of 0.01—0.5 μg/mL, with regression coefficient of 0.9995 and detection limit of 0.006 μg/mL. This simple and sensitive method has been successfully applied to determine cimetidine in tablets and capsules, with average recovery of (98.47±0.92)% and (97.07±1.16)%, respectively. Furthermore, the mole ratio of the complex between cimetidine and 1,5-dichloroanthraquinone is 2∶1, and the mechanism of charge-transfer reaction is explored.  相似文献   
4.
Three methods were used to immobilize myoglobin (Mb) on chitosan/single-wall carbon nanotubes (SWNTs) film, and direct electrochemistry of the immobilized Mb was extensively investigated. Immobilized Mb displayed a couple of stable and well-defined redox peaks with the formal potential (E’) is at about −0.27 V (vs. SCE) in 0.1 M phosphate buffer solution (pH 7.0). The E′ was shifted linearly with pH in the range of 3.0 to 9.0 with a slope of −54.1 mV pH−1, denoting that one-electron accompanies with one-proton transfer in electrode reaction process. The FT-IR spectroscopy and UV-vis spectroscopy showed that Mb on the film retained its secondary structure similar to its native state. The experimental results demonstrated that the immobilized Mb exhibited excellent electrocatalytic activity to reduction of cimetidine with a significant lowering of overpotential. The electrocatalytic current was proportional to the concentration of cimetidine over the range from 9.80 × 10−6 to 1.1 × 10−4 M; the detection limit is 8.40 × 10−6 M (signal-to-noise ratio of 3). The proposed method exhibits good sensitivity, stability and reproducibility. Published in Russian in Elektrokhimiya, 2008, Vol. 44, No. 2, pp. 235–243. The text was submitted by the authors in English  相似文献   
5.
在弱碱性的多聚磷酸钠介质中,二价铜离子、过氧化氢和染料罗丹明B混合可以产生较强的化学发光,西咪替丁对此发光有较强的抑制作用,其抑制发光强度与西咪替丁P43的质量浓度在5.0-1000μg.L-1范围内呈良好的线性关系,基于此,结合流动注射技术,建立了一种直接测定西咪替丁的化学发展发光新方法。该方法具有较高的灵敏度,检出限为2.2μg.L-1(IUPAC),对500μg.L-1西咪替丁平行测定11次,其相对标准偏差为2.1%。该方法已成功用于西咪替丁胶囊和针剂含量的测定。  相似文献   
6.
The World Health Organization issued a nitrosation procedure (NAP Test) which allows to carry out nitrosation under standard conditions. It has proved that the in vitro reaction rates of the fast nitrosatable drugs piperazine, cimetidine and ethambutol are not influenced by -, - and -cyclodextrin. On the contrary, -, -cyclodextrin and heptakis-2,6-di-O-methyl--cyclodextrin enhance the nitrosation of the slower nitrosatable 1-ephedrine and fencamfamine significantly. This possible reaction must be considered if nitrosatable drugs are formulated with cyclodextrins to be administered to human beings.  相似文献   
7.
TG and DSC data were used to determine the thermal parameters of metronidazole drug and tablets. Three tablets A, B and C were analysed. The TG curves of metronidazole drug and tablets A and B displayed five and C four thermal decomposition processes, respectively. Analysis of the DSC data pointed to chemical interactions between metronidazole drug and the excipients of tablets, suggested by alterations in the melting point of metronidazole. The rate constants obtained from the isothermal TG data presents following sequence of the thermal stability: tablet A>tablet C>metronidazole drug>tablet B. This revised version was published online in July 2006 with corrections to the Cover Date.  相似文献   
8.
This work developed a methodology that can potentially be applied to the quality control of cimetidine drug substance and its tablets. The kT obtained at different temperatures (200, 190, 180, 170 and 160°C) were determined by isothermal thermogravimetric method using the classical Arrhenius equations. The dissolution profiles were obtained using USP 24 (Method 711) and rate constants (kD) were determined by Kitazawa equations. An evaluation was made to check if there was statistically significant correlation between the two variables kT and kD. Isothermal TG data were used to determine the reaction order and degradation reaction rate constants. The results showed that in all temperatures thermal order (kT) was: C<A<B tablets, while dissolution order (kD) was: C<A<B tablets. In conclusion, correlation between kT/kD seems to be a suitable method for detecting possible interactions between cimetidine and excipients in development or manufacturing changes, particularly for immediate release dosage forms and therefore could be especially useful on quality control. This revised version was published online in July 2006 with corrections to the Cover Date.  相似文献   
9.
悬浮聚合法制备西咪替丁印迹聚合物微球的分子选择性能   总被引:14,自引:0,他引:14  
以西咪替丁为印迹分子,2-丙烯酰胺-2-甲基丙磺酸(AMPS)为功能单体,三羟甲基丙烷三甲基丙烯酸甲酯(TRIM)为交联剂,采用悬浮聚合法制备得到了平均粒径在60-310μm之间的分子印迹聚合物微球(MIPMS),将所得的MIPMS用作固相萃取剂(SPE)的测试结果表明,该MIPMS对西咪替丁有较好的特异选择性能,当以苯丙氨酸为竞争分子时,分离因子可达1.75,且该MIPMS呈现出较好的再生性。而未印迹的空白聚合物则无此分子选择性。  相似文献   
10.
This study demonstrates the analysis of cimetidine in human plasma with HPLC using a simplified sample preparation by protein precipitation with perchloric acid. Plasma cimetidine concentration was determined by plotting peak height ratio of cimetidine to ranitidine (internal standard, IS) against cimetidine concentrations in plasma. The cimetidine and ranitidine peaks were completely separated and no interference from plasma was observed. The lower limit of quantification (LLOQ) of the method was established at 0.1 microg/mL with a precision of 4.3% and a relative error of 1.9%. The average analytical recovery was >90% over the range of cimetidine concentrations (0.1-15.0 microg/mL). The linearity of calibration curve was excellent (r(2) > 0.999). The within- and between-day precision and accuracy, expressed as the coefficients of variation and relative error, were found to be less than 5%. Compared with previously reported methods, the analytical technique for cimetidine determination in human plasma presented here demonstrates comparable accuracy and precision, an acceptable analysis time, shorter and simpler sample preparation, and a reduced need for complicated equipment. The method presented here is simple and rapid, and the precision and sensitivity are appropriate for the determination of cimetidine in plasma in pharmacokinetic studies.  相似文献   
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