流动注射联用技术在药物分析中的应用进展

流动注射分析具有分析速度快、灵敏度高、自动化程度高等优点,可以与多种检测器联用,如紫外-可见检测器、荧光检测器、化学发光检测器、电化学检测器等,本文综述了流动注射联用技术在药物分析中的应用进展。     

Flow injection analysis: a new approach to pharmaceutical determinations

A review is presented in which the fundamental principles, instrumentation and practical aspects of flow injection analysis (FIA) are discussed. A particular focus is put on applications in pharmaceutical chemistry, which offers a wide scope to the new technique.     

Novel flow injection analysis systems for drug analysis

Flow injection analysis (FIA) has become a versatile tool for rapid and automated analyses. As its capabilities have increased, so have the complexity and operation of the apparatus. We have been investigating ways to simplify both the apparatus and the application of injection techniques. A novel cam-driven syringe pump and the development of sequential injection analysis (SIA) are reviewed, and some applications presented. Flow injection coulometric titrations are presented as a means to further alleviate reagent stability and calibration problems. These systems have potential for automatically carrying out many drug assays.     

Flow injection analysis of pharmaceuticals

An overview of the most representative problems solved by flow injection analysis (FIA) in drug analysis is presented. Different aspects of this technique which can be manipulated with specific purposes are discussed and special emphasis is placed on the possibilities of FIA in dissolution test control.     

FIA法测定Vc片的含量

本文报道Vc片与1,10-菲咯啉铁(Ⅲ)形成有色络合物在510nm处有最大吸收,利用流动注射分析法测定其含量。标准曲线相关系数为0.9999,两个批号样品测定结果含量分别为标示量的94.4%和97.3%,变异系数分别为0.26%(n=6)和0.19%(n=6),平均回收率为99.8%,与中国药典(1985年版)相比,F检验(F_计=1.88相似文献   

Binding study of drug with bovine serum album using a combined technique of microdialysis with flow-injection chemiluminescent detection

Microdialysis coupled with flow-injection chemiluminescence (FI–CL) has been developed to determine the binding parameters of a drug binding to protein by using antibiotic tetracycline hydrochloride binding to bovine serum albumin as a model system. The drug and protein were mixed in different molar ratios in 0.067 M phosphate buffer, pH 7.4, and incubated at 37 °C in a water bath. The microdialysis probe was utilized to sample the mixed solution at a perfusion rate of 5 μL/min. The concentration of unbound tetracycline hydrochloride in the microdialysate was determined by FIA–CL. In vitro recovery of tetracycline hydrochloride under experimental conditions was 30.0%. The data obtained by the present microdialysis–FI–CL system was analyzed using the Scatchard analysis and Klotz plot. The results show that the Scatchard plot and Klotz plot are linear with good correlation coefficient, indicating a good agreement of the experimental data and to the theoretical equation. The FIA chemiluminescence system combined with microdialysis developed in this work demonstrated its use for determination of interaction between drug and protein by using relatively simple instrument.     

Flow-injection inhibition chemiluminescence determination of indapamide based on luminol-ferricyanide reaction

A novel and sensitive chemiluminescence (CL) method for the determination of indapamide coupled with flow-injection analysis (FIA) technique is developed in this paper. It is based on the inhibition effect of the studied drug on the chemiluminescence emission of luminol-potassium ferricyanide system. Under the optimum conditions, the decreased CL intensity is proportional with the concentration of indapamide in the range of 1 x 10(-8) to 1.0 x 10(-6) g ml(-1). The detection limit is 3.4 x 10(-9) g ml(-1) (3sigma). A complete analysis could be performed in 45 s including washing and sampling, giving a throughout of about 90 h(-1). The relative standard deviation (R.S.D.) for 11 parallel measurements of 1.0 x 10(-7) g ml(-1) indapamide is 3.0%. The proposed method has been applied for the determination of indapamide in its pharmaceutical formulations. The results obtained compared well with those by an official method. The possible inhibition mechanism of indapamide on luminol-potassium ferricyanide CL system was discussed briefly.     

Chemiluminescence determination of sulphadiazine in drugs by flow injection analysis using the peroxyoxalate reaction in micellar medium

Peroxyoxalate chemiluminescence (PO-CL) is an indirect type of CL which allows the detection of native fluorophores or compounds derivatized with fluorescent labels. We propose a flow injection analysis (FIA) configuration based on the use of a two-injection valve system for the introduction of both PO and derivatized analyte solutions in the flow system, avoiding the problems arising from the use of organic solvents, such as acetonitrile, as no special tubes nor special pumps are required. Furthermore, the use of micellar media (sodium dodecyl sulphate, SDS) as a carrier and the addition of tetrahydrofurane (THF) in the PO solutions increase both the solubility and stability of POs, avoiding their rapid degradation in water. The proposed CL-FIA system has been applied to the determination of sulphadiazine (a sulphonamide mainly used in the treatment of urinary tract infections for human and veterinary use) using bis[2,4,6-trichlorophenyl]oxalate (TCPO) as CL precursor, H2O2 as oxidant, imidazole as a catalyst and fluorescamine as the fluorescent derivatizing agent. The optimization of variables was carried out by means of experimental designs and the method showed a LOQ of 379 microg l(-1) (calibration range 126-2000 microg l(-1)). It has been satisfactorily applied to the quantification of sulphadiazine in pills for human use and ampoules for veterinary use.     

Towards disposable sensors for drug quality control: Dextromethorphan screen‐ printed electrodes

A simple, rapid, reliable, and reproducible method for mass production of disposable sensors using screen‐printing technology is described. Homemade printing has been characterized and optimized on the basis of effects of the modifier and plasticizers. The fabricated bi‐electrode potentiometric strip containing both working and reference electrode was used as dextromethorphan (DXM) sensor. The proposed sensors worked satisfactorily in the concentration range from 10^?5 to 10^?2 mol L^?1 with detection limit reaching 6 × 10^?6 mol L^?1 and adequate shelf life of 8 months. DXM was determined in pharmaceutical formulations under batch and flow injection analysis (FIA) conditions with sampling output 120 h^?1. Copyright © 2010 John Wiley & Sons, Ltd.     

气相色谱-质谱联用结合化学计量学分辨法分析甘松的挥发油成分

目的分析中药甘松的挥发油成分。方法采用气相色谱-质谱联用(GC-MS)结合化学计量学分辨法对甘松挥发油成分进行定性分析,对重叠峰和包埋峰采用直观推导式演进特征投影法(HELP)和选择离子法(SIA)进行分辨,同时计算各组分的程序保留指数(PTRI),用NIST质谱库对解析后的纯组分进行定性。结果定性分析出69种化学成分,占总含量的93.98%。结论GC-MS法结合化学计量学分辨法比单用GC-MS法定性结果更加准确、可靠。     

Chemiluminescence detection of opium poppy (Papaver somniferum) alkaloids

A review with 98 references. The determination of the opium poppy (Papaver somniferum) alkaloids and their semi-synthetic derivatives has important applications in industrial process monitoring, clinical analysis and forensic science. Liquid-phase chemiluminescence reagents such as tris(2,2'-bipyridyl)ruthenium(II) and acidic potassium permanganate exhibit remarkable sensitivity and complementary selectivity for many P. somniferum alkaloids, which has been exploited in the development of a range of analytical procedures using flow analysis, high-performance liquid chromatography, capillary electrophoresis and microfluidic instrumentation.     

FIA determination of chlorhexidine by means of the precipitation with Cu(II)

The determination of chlorhexidine in pharmaceutical formulations is carried out using flow injection analysis (FIA) with measurement by atomic absorption spectrometry (AAS). The method is based on the formation of a copper—biguanide complex precipitate when the sample is injected into an ammoniacal copper solution. The precipitate is retained on a plastic or paper filtering device. A nitric acid stream dissolves the precipitate and carried the Cu(ll) to the AAS detector. The chlorhexidine is determined over the range 5–20 ppm. The influence of interfering substances is investigated.     

Enzymatically modified ion-selective electrodes for flow injection analysis

The application of potentiometric biosensors based on membrane ion-selective electrodes for flow injection analysis (FIA) is presented. The biosensors have been obtained by covalent binding of enzyme molecules directly to surface of ion-selective membranes. The biosensor/FIA systems enable the determination of urea and penicillin in the millimolar ranges of concentration. About 30 samples per hour can be analysed in the performed FIA systems. The operational stability of the bioanalytical systems exceeds 1 month.     

Determination of dopamine by flow-injection analysis coupled with luminol-hexacyanoferrate(III) chemiluminescence detection

A novel flow-injection method (FIA) for the determination of dopamine based on the inhibition of the intensity of chemiluminescence (CL) from luminol-hexacyanoferrate(III) system in basic medium is described. The present method allows the determination of dopamine over the range 30-100 microg l(-1) and 400-3000 microg l(-1). The relative standard deviation is 2.32% for 70 microg l(-1) dopamine and 1.22% for 1500 microg l(-1) dopamine (n = 20). The detection limit is 5 microg l(-1) with the sampling rate of 135 samples h(-1). This method has been applied for the determination of dopamine in commercial pharmaceutical injection samples. The results obtained by this method agreed with those by the official method.     

Determination of cefmetazole residue at pharmaceutical manufacturing facilities by chemiluminescence flow injection analysis

Application of a sensitive and rapid flow injection analysis (FIA) method with luminol chemiluminescence detection for determination of trace amounts of cefmetazole (CMZ) in cephamycin antibiotic residue in pharmaceutical manufacturing facilities and on pharmaceutical manufacturing equipment has been investigated. The method was shown to be sensitive at a level of limit of detection of 0.06 ng/ml and for linear concentrations in the range of 0.3-1.5 ng/ml. Average recoveries of CMZ from stainless steel plates and glass plates were 62.1% and 60.1%, respectively, by adding 15 ng/100 cm2, and that of air sampling filters was 91.9% by adding 3 ng/filter. The proposed method has been successfully applied to the determination of CMZ residue in samples collected from an actual manufacturing facility and equipment. According to the results, no detectable CMZ residue was observed, therefore it was verified that no contamination had occurred to other pharmaceutical products manufactured in the facility.     

FIA determination of ascorbic acid at low potential using a ruthenium oxide hexacyanoferrate modified carbon electrode

The anodic oxidation of ascorbic acid on a ruthenium oxide hexacyanoferrate modified electrode was characterized by cyclic voltammetry. On this modified surface, the electrocatalytic process allows the determination of ascorbic acid to be performed at 0.0 V and pH 6.9 with a limit of detection of 2.2 microM in a flow injection configuration. Under this experimental condition, no interference from glucose, nitrite and uric acid was noticed. Lower detection limit values were obtained by measuring flow injection analysis (FIA) responses at 0.4V (0.14 microM), but a concurrent loss of selectivity is expected at this more positive potential. Under optimal FIA operating conditions, the linear response of the method was extended up to 1 mM ascorbic acid. The repeatability of the method for injections of a 1.0 mM ascorbic acid solution was 2.0% (n=10). The usefulness of the method was demonstrated by an addition-recovery experiment with urine samples and the recovered values were in the 98-104% range.     

Comparison of a fluorescent immunoassay with an enzyme immunoassay and a radioimmunoassay for gentamicin

A fluorescent immunoassay (FIA) for gentamicin was evaluated and compared with an enzyme multiplied immunoassay (EMIT) and a radioimmunoassay (RIA) for gentamicin. Pooled human serum that contained low, medium, and high concentrations of gentamicin sulfate (approximately 2.5, 5, and 10 micrograms/ml of gentamicin) were analyzed for actual gentamicin concentration by FIA. Samples were assayed 10 times during the same day to evaluate within-run precision and on 10 different days to evaluate between-run precision. Serum samples obtained from patients receiving gentamicin therapy were analyzed for gentamicin concentration using FIA and EMIT, and separate serum samples were analyzed using FIA and RIA. Results were compared by regression analysis. Within-run coefficients of variation were 8.47%, 6.84%, and 2.62%, respectively, for the low, medium, and high concentrations of gentamicin, and the respective between-run coefficients of variation were 10.81%, 6.31%, and 1.64%. The correlation coefficient for the comparison of FIA with EMIT was 0.943, and the correlation coefficient for the comparison of FIA with RIA was 0.970. The fluorescent immunoassay is a reliable method for determining the concentration of gentamicin in serum. Although the results obtained by FIA correlate well with those obtained by EMIT and RIA, variability exists between concentrations determined by each of these methods.     

化学发光微粒免疫分析法对心肌损伤标志物及BNP检测的方法学性能评价

目的 用化学发光微粒免疫分析(CMIA)法测定血浆B型钠尿肽(BNP)和血清肌钙蛋白(TPI)、肌红蛋白(MYO)、肌酸激酶(CKMB),从而了解其检测性能.方法 用雅培公司的i2000SR化学发光分析仪,对该方法的精密度、准确度、线性、抗干扰能力、携带污染率、灵敏度进行评价,并验证各项目的参考值区间.结果 (1) ...     

Suppressive effect of sialic acid on the prostaglandin E2-mediated edema in carrageenin-induced inflammation of rat hind paws]

We performed these studies to determine whether sialic acid (SIA) existed in the inflammatory exudate of the carrageenin (Car)-air pouch model and to elucidate the mechanisms of the antiinflammatory action of SIA on the Car-induced edema in rat hind paws. SIA (113.20 +/- 10.73 micrograms/ml) was detected in the exudate of Car-air pouch, and the plasma SIA (660.29 +/- 29.38 micrograms/ml) in Car-air pouch rats was significantly higher than that (490.00 +/- 29.37 micrograms/ml) in control rats. SIA (300 mg/kg, s.c.) suppressed the delayed phase of Car-induced edema, and it also suppressed the edema induced by Car plus arachidonic acid, Car plus PGE2, and bradykinin plus PGE2. However, SIA did not affect the edema induced by dextran, histamine, bradykinin, and Car plus PGE1. SIA affected neither the PG production in rats nor the [3H]PGE2-receptor binding of guinea pig ileum, and SIA reduced the PGE2-induced contraction of isolated guinea pig ileum. The above results suggest that SIA induces the antiinflammatory effects via its antagonism against PGE2. Furthermore, the presence of SIA in the inflammatory exudate and the higher concentration of SIA in the plasma than in the exudate might suggest that SIA plays patho-physiologically protective roles in inflammatory states.     

Comparison of different flow injection approaches to the automatic determination of enzymatic activity

Three configurations based on the principles behind flow injection analysis (FIA) are proposed for the automatic determination of enzymatic activity. The proposed approaches are normal, stopped-flow and open-closed FIA. The comparative study of the methods developed from these approaches allows the establishment of the scope of the application of each, with inherent advantages and disadvantages.