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41.
42.
Novel techniques have recently emerged to separate chiral drug compounds into pure enantiomers. The mechanism, experimental difficulties, and applicability of these methods can vary greatly, and the choices involved are not straightforward. The most significant new advances in the field of chiral separations have come from work done with liquid chromatographic systems and chiral stationary-phase columns. This review describes several commonly used approaches to chiral separation, diastereomeric derivatization, chiral mobile-phase additives, and three major types of chiral stationary phases. Although no single method can be judged superior for every drug application, it appears that chiral stationary phases have received the most attention recently and they are emphasized here. 相似文献
43.
Summary A new gas-liquid chromatographic (GLC) determination of cholesterol sulfate (CS) and dehydroepiandrosterone sulfate (DHEAS) for a biochemical diagnosis of recessive X-linked ichthyosis (RXLI) is described. Although the GLC method for determination of CS is known to be more sensitive than the thin layer chromatographic (TLC) method, the former method has not been widely employed because of its complicated pre-purification steps. The present method allows us to measure the serum levels of CS and DHEAS without tedious purification steps such as multiple conventional column chromatography and preparative thin layer chromatography. Sulfated steroids are rapidly purified with a commercially available mini disposable cyclohexylsilane-bonded phase (CH) column, CH BOND ELUT, and the purified steroids after desulfation are converted to water-resistant tert-butyldimethylsilyl ether derivatives for the GLC analysis on dual 2 m glass columns packed with 2% XE-60 on Chromosorb W.By the present method, serum CS concentrations in RXLI patients were shown to be about 10 times higher than those in patients with ichthyosis vulgaris, carriers of RXLI, and healthy subjects. This method is more suitable not only for a biochemical diagnosis of RXLI but also for studies on the metabolism of sulfated steroids than the previous time-consuming GLC methods. 相似文献
44.
Purpose. To obtained rate constants from weight-averaged (Mw) or z-averaged (Mz) molecular weights for polymers of Schule-Flory distribution and undergoing random scission. These constants were compared with those obtained by parallel 1HNMR studies.
Methods. The hydrolysis of two poly(ortho ester)s were followed by 1HNMR and gel permeation chromatography (GPC).
Results. Equations to convert number-averaged (Mn), Mw and Mz into fraction of backbone remaining (fc) were derived. First-order hydrolytic rate constants of two poly(ortho ester)s; DETOSU-HD and DETOSU-CDM were calculated using these relationships. The rate constants calculated from 1HNMR, Mz and Mw were 0.215, 0.218 and 0.182 hr–1, respectively, for DETOSU-CDM and 0.152, 0.086 and 0.038 hr–l for DETOSU-HD. The large discrepancy in the rates determined by 1HNMR and GPC in the latter case was attributed to that the detector response (refractive index) of the monomers was lower than that of the high molecular weight polymer. The difference is small in the case of DETOSU-CDM, and the rates calculated from GPC data were comparable or nearly identical to that obtained from 1HNMR data.
Conclusions. Although GPC can yield rapid and valuable kinetic data for the degradation of biodegradable polymers, the system, however, must be carefully calibrated to account for the variations in Mark-Houwink coefficients and in the response of the mass detector between the high and low MW polymers. 相似文献
45.
46.
Changes in the content of the opiate peptide Met-enkephalin at the early stages of immune response are studied in different
structures of rats brain 20 min and 24 h after immunization with sheep erythrocytes.
Translated fromByulleten’ Eksperimental’noi Biologii i Meditsiny, Vol. 123, No. 2, pp. 170–172, February, 1997 相似文献
47.
A method based on ion-exchange column chromatography to enhance the protein content of fruit allergenic extracts was found to help make the subsequent SDS-PAGE immunoblotting assays possible; otherwise, they were difficult to achieve due to the high carbohydrate content. Fractionated extracts of apple, pear, and peach (peel and pulp) were obtained by anion-exchange chromatography (Q-SepharoseTM column), providing clear electrophoretic patterns which allowed IgE detection by enzymatic assays of the transferred membranes. This chromatographic method produced in one single step an enriched extract directly from the standard crude aqueous one, with an increment in the protein content of more than sixfold, on average; thus, it proved to be more suitable than the usual chemical fractionation procedures. 相似文献
48.
胶束电动毛细管色谱法测定复方酮康唑霜中酮康唑和特美呋的含量 总被引:1,自引:0,他引:1
目的:毛细管电泳法测定酮康唑霜中酮康唑和特美味的含量。方法:分离缓冲液为胆汁酸钠(70 mmol/L)-三羟甲基氨基甲烷-磷酸(50 mmol/L)(pH 8.14),分离电压30 kV、温度25 C、50 μm(内径)×48.5cm(有效长度40cm)空心熔融石英毛细管柱、检测波长240nm。结果:以丙酸睾酮为内标,酮康唑质量浓度在140.5~702.5 μg/ml、特美呋质量浓度在151~755μg/ml之间成良好的线性关系;加样回收率分别为95.4%~103.9%、95.9%~102.6%,RSD%分别为2.8%~4.2%(n=3)、2.9%~3.6%。结论:本法简便、快速、可靠,可用于该复方制剂中酮康唑及特美呋的含量测定。 相似文献
49.
Jaroslav Salamoun Jo
rg Remien 《Journal of pharmaceutical and biomedical analysis》1992,10(10-12):931-936
The inhibiting compounds were separated by micro-column liquid chromatography in the mobile phase containing the natural substrate acetylcholine. A home-made packed bed microbioreactor system containing immobilized enzyme acetylcholinesterase (ACHE) in human red blood cell membrane and choline oxidase (CHO) from alcaligenes was used for the post-column conversion of acetylcholine to hydrogen peroxide which was detected by an electrochemical detector. The inhibition effect of the solutes caused a decrease in the acetylcholinesterase activity, a decrease in the formation of hydrogen peroxide and also a decrease in the response corresponding to the concentration of the solutes. The rate of the enzyme regeneration was also recorded. The micro-system was compared with a conventional LC system comprising commercially prepared enzyme reactor. The stability of the enzymes is at least 3 weeks at ambient temperature. The limit of detection depends on biological activity of inhibition and for galanthamine was 1 pmol. 相似文献
50.
采用气相色谱法,以尼莫地平为内标测定钙拮抗剂异硝苯地平。方法简便快速,结果准确可靠。回收率99.78%,相对标准偏差0.43%,符合定量测定的要求。 相似文献