Rapid determination of subnanogram urapidil using flow injection enhancement chemiluminescence

A sensitive flow-injection (FI) chemiluminescence (CL) for the determination of urapidil is described in this paper. It is based on the enhancement effect of urapidil on the CL reaction between luminol and hydrogen peroxide. The increment of CL intensity is proportional to the concentration of urapidil in the range 0.1−10 ng/mL (R ²=0.9986), with a detection limit (3σ) of 0.03 ng/mL. The whole process, at a flow rate of 2.0 mL/min, including sampling and washing, could be completed in 0.5 min, and the relative standard deviation (RSD) at the concentration of 0.1, 1.0, and 10.0 ng/mL was less than 3.0% (n = 5). The proposed method has been successfully applied for the determination of urapidil in pharmaceutical preparation, human urine, and serum. The text was submitted by the authors in English.     

A simple flow-injection chemiluminescence method for the determination of trace pentavalent vanadium in water samples

A simple method for rapid determination of trace pentavalent vanadium in natural water was presented by flow-injection chemiluminescence (CL). Through water injection, luminol and potassium permanganate were eluted from the anion exchange column to generate the CL, which was enhanced in the presence of V(V). Under the optimum conditions, the increased CL intensity was linear with V(V) concentration in the range from 0.1 to 100?ng?mL^?1. The limit of detection was 50?pg?mL^?1 (3σ) and the relative standard deviation (RSD) was 2.24% (n?=?5) for a 1.0?ng?mL^?1?V(V). At a flow rate of 2.0?mL?min^?1, one cycle of analysis could be performed in 0.5?min with a RSD of less than 3.0%. The proposed method was successfully applied to the determination of vanadium in natural water.     

Determination of Biotin in Pharmaceutical Formulations by Potassium Permanganate-luminol-CdTe Nanoparticles Chemiluminescence System

A sensitive flow-injection chemiluminescence method was developed for the determination of biotin in the pharmaceutical formulations. The affinity between avidin and biotin was used to adsorb biotin on the polystyrene, with subsequent quantification of biotin based on its ability to enhance the chemiluminescence(CL) signal generated by the redox reaction of potassium permanganate-luminol-CdTe nanoparticles CL system. The investigations prove that apart from 3-aminophthalate, the CdTe quantum dots(QDs) play both catalytic and emitter roles. Under optimum conditions, the linear range for the determination of biotin was 0.01-25ng/mL with a detection limit of 7.3?10^-3 ng/mL(S/N=3). The relative standard deviation of 5 ng/L biotin was 2.06%(n=7). The proposed method was used to determine the biotin concentration in the pharmaceutical formulations and the recovery was between 96.4% and 104%. The proposed method is simple, convenient, rapid and sensitive.     

Quantitative Monitoring of Rutin in Human Urine by Flow Injection‐Chemiluminescence Analysis

In this paper, a rapid and sensitive flow injection‐chemiluminescence (FI‐CL ) method is proposed for the quantitative determination of rutin based on the inhibitory effect of rutin on the chemiluminescence intensity from the luminol–chymotrypsin (CT ) system. The decrease of CL intensity was found to be proportional to the logarithm of rutin concentration in the range 0.1–30.0 ng/mL . A method for the quantification of rutin is proposed, with the limit of detection (LOD ) of 0.03 ng/mL (3σ). A complete analytical process including sampling and washing for rutin determination, which was conducted at a flow rate of 2.0 mL /min, could be performed completely within 30 s, yielding a sample efficiency of 120 h⁻¹. The proposed procedure was successfully applied for the determination of rutin in human urine after oral intake, with recoveries varying from 93.9 to 108.1% and relative standard derivation <4.0% (n = 5). Results showed that urine reached the maximum concentration at ~2.5 h, and the total excretion ratios were (83.5 ± 0.6) and (86.8 ± 0.7)%, respectively, for two volunteers in 8 h. The pharmacokinetic parameters, including the half‐life (1.05 ± 0.02 h), absorption rate constant (1.18 ± 0.01 h⁻¹), and elimination rate constant (0.70 ± 0.01 h⁻¹), were obtained. The possible CL mechanism of the luminol–CT –rutin reaction is discussed by FI‐CL , fluorescence, and molecular docking methods.     

Flow Injection Chemiluminescence Determination of Prednisone Acetate by Oxidation with N-Bromosuccinimide

A simple flow injection chemiluminescence (CL) method for the determination of prednisone acetate was developed. This method is based on the fact that the strong CL of N-bromosuccinimide (NBS) and calcein can be inhibited by prednisone acetate. The CL intensity correlated linearly with the concentration of prednisone acetate over the ranges of 0.02–0.4 mg/L and 0.4–10 mg/L. The CL mechanism was also proposed. The detection limit (3σ) of prednisone acetate was 13 ng/mL and the relative standard deviation was 1.3% at 0.1 mg/L prednisone acetate (n = 11 measurements). This method was applied to the determination of prednisone acetate in the tablets with good results.     

Gold nanoparticle-based immunoassay by using non-stripping chemiluminescence detection

A novel microplate-compatible chemiluminescence (CL) immunoassay has been developed for the determination of human immunoglobulin G (IgG) based on the luminol-AgNO(3)-gold nanoparticles CL system. Polystyrene microtiter plates were used for both immunoreactions and CL measurements. The primary antibody, goat-anti-human IgG, was first immobilized on polystyrene microwells. Then the antigen (human IgG) and the gold-labeled second antibody were connected to the microwells successively to form a sandwich-type immunocomplex. The gold label could trigger the reaction between luminol and AgNO(3), accompanied by light emission. Under the optimized conditions, the CL intensity of the system was linear with the logarithm of the concentration of human IgG in the range from 25 to 5000 ng mL(-1), with a detection limit of 12.8 ng mL(-1) ( approximately 80 pM) at a signal to noise ratio of three (S/N = 3). Compared with other reported CL immunoassay method based on gold labels, the proposed CL protocol avoids a strict stripping procedure or difficult to control synthesis processes, making the method more simple, time-saving and easily automated. The present CL method is promising for the determination of clinically important bioactive analytes.     

Determination of phenothiazines in pharmaceutical formulations and human urine using capillary electrophoresis with chemiluminescence detection

A CE instrument coupled with chemiluminescence (CL) detection was designed for the determination of promethazine hydrochloride (PTH) and promazine hydrochloride (PMH) in real samples. An important enhancement of the CL emission of luminol with potassium ferricyanide was observed in the presence of these phenothiazines; so this system was selected for their detection after CE separation. Parameters affecting the electrophoretic separation were optimized in a univariate way, while those affecting CL detection were optimized by means of a multivariate approach based on the use of experimental designs. Chemometrics was also employed for the study of the robustness of the factors influencing the postcolumn CL detection. The method allows the separation of the phenothiazines in less than 4 min, achieving LODs of 80 ng/mL for PMH and 334 ng/mL for PTH, using sample injection by gravity. Electrokinetic injection was used to obtain lower LODs for the determination of the compounds in biological samples. The applicability of the CE-CL method was illustrated in the determination of PTH in pharmaceutical formulations and in the analysis of PMH in human urine, using a previous SPE procedure, achieving an LOD of 1 ng/mL and recoveries higher than 85%.     

Flow‐Injection Chemiluminescence Analysis of Cloperastione Hydrochloride

Abstract

A new chemiluminescence (CL) reaction was observed when cloperastine hydrochloride was injected into the reaction mixture after the CL reaction of Ce(IV) and sodium sulfite finished. A new flow injection CL method for the determination of cloperastine hydrochloride was established based on the CL reaction. The relative standard deviation (RSD) for the determination of cloperastine hydrochloride was 1.3% (n=11, c=1.0×10^?6 g/mL). The CL intensity responded linearly to the concentration of cloperastine hydrochloride in the range 2.0×10^?7～2.0×10^?5 g/mL (r=0.9962). The detection limit was 5×10^?8 g/mL cloperastine hydrochloride. The method had been applied to the determination of cloperastine hydrochloride in tablets with satisfactory results.     

Sensitive determination of phenothiazines in pharmaceutical preparation and biological fluid by flow injection chemiluminescence method using luminol-KMnO4 system

A flow injection chemiluminescence method was described for the determination of four phenothiazine drugs, namely, chlorpromazine hydrochloride, perphenazine hydrochloride, fluphenazine hydrochloride and thioridazine hydrochloride. Strong Chemiluminescence (CL) signal was produced when above-mentioned drug was injected into the mixed stream of luminol with KMnO₄. The linear ranges of the method were 0.0020-1.0 μg/mL chlorpromazine hydrochloride, 0.0040-3.0 μg/mL perphenazine hydrochloride, 0.0020-5.0 μg/mL fluphenazine hydrochloride and 0.0050-1.0 μg/mL thioridazine hydrochloride. The detection limits were 0.4 ng/mL chlorpromazine hydrochloride, 0.7 ng/mL perphenazine hydrochloride, 2 ng/mL fluphenazine hydrochloride and 0.7 ng/mL thioridazine hydrochloride. The proposed method was applied to the determination of chlorpromazine hydrochloride in injections and in mental patient's urine samples and the satisfactory results were achieved. The possible CL reaction mechanism was also discussed briefly.     

Determination of vitamin B<Subscript>12</Subscript> using a chemiluminescence flow system

A method to determine vitamin B₁₂ by measuring the chemiluminescence (CL) intensities using a flow injection (FI) system has been proposed. It is based on the catalytic effect of cobalt(II) in vitamin B₁₂ on the CL reaction between luminol and hydrogen peroxide in a basic medium. The increment of the CL intensity is proportional to the concentration of vitamin B₁₂ in the range 8.68–86.9 ng/mL (r ² = 0.9984) with a detection limit (3σ) of 0.89 ng/mL. The CL response is obtained in 10 s at a flow rate of 3.0 mL/min with a relative standard deviation (RSD) of less than 2.5% (n = 6). The method has been successfully applied to the determination of vitamin B₁₂ in pharmaceutical injections. The text was submitted by the authors in English.     

Determination of matrine in medicine and bio-fluids based on inhibition of luminol-myoglobin chemiluminescence

A green, rapid and sensitive flow injection procedure based on the inhibition of the chemiluminescence (CL) intensity from the luminol-myoglobin (Mb) system is proposed for the determination of matrine. The decrement of CL signal was linear with the logarithm of the matrine concentration over the range from 10 to 1000 ng/mL (R ² = 0.9978) offering a detection limit of 3.5 ng/mL. At a flow rate of 2.0 mL/min, one analysis cycle, including sampling and washing, could be accomplished in 0.5 min with a relative standard deviation (RSD) of less than 5.0%. The sensitive flow injection method was successfully applied to the determination of matrine in pharmaceutical injection and human serum, with recoveries from 94.1 to 113.4% and RSDs of less than 5.0%.     

Chemiluminescence Determination of Molybdenum by on-Line Reduction with a Flow Injection System

ThereactionsofLuwithhydrogenperoxidecatalysedbymetalionsandalsoreactionofLuwithorganicreductantssuchasglucoseandascorbicacidhavebeenreported"=.OurrecentstudiesshowedthatsomeinorganicreductantssuchasMo(Ill),V(11),U(ill),W(ill),Cr(II),Ti(ill)andFe(11)etc.canreactwithLuinstrongalkalinemediumtogenerateCL.Inthispaper,theCLreactionbetweenLuandMo(ill)producedbyaJonesreductor3hasbeenstudiedindetailforthefirsttime,andtheCLreactionhasbeensuccessfullyappliedtodeterminemolybdenumwithexcellentsensi…     

Simultaneous chemiluminescent determination of carbaryl and 1-naphthol in soils using a flow-injection system

A flow-injection method coupled with the luminol chemiluminescence (CL) detection was developed for the simultaneous determination of carbaryl and 1-naphthol in soils. The method is based on the inhibition of luminol oxidation by the presence of 1-naphthol with the consequent reduction in the CL intensity. The conversion of carbaryl into 1-naphthol was made by the alkaline hydrolysis with NaOH. Under the optimised conditions, the method permits the determination of carbaryl and 1-naphthol over the range 25–400 ng mL^?1 with high determination coefficient using both peak area and height, and high sample throughput (40 h^?1). The detection limits applying the International Unión of Pure and Applied Chemistry (IUPAC) criteria were 65 ng g^?1 and 123.5 ng g^?1 for peak height and area, respectively. A simple extraction procedure employing chloroform as the solvent and sonication was effective for the complete extraction of the analytes present in soils. The method was validated by the analysis of spiked samples, with recoveries between 88.7 and 103.1%. The Flow Injection-Chemiluminescence (FI-CL) method has proven to be simple, fast and accurate for the quantification of carbaryl and its main degradation product in soils.     

Flow chemiluminescence sensor for determination of clenbuterol based on molecularly imprinted polymer

In this paper, a novel flow chemiluminescence (CL) clenbuterol sensor based on molecularly imprinted polymer (MIP) on line enrichment nanogram clenbuterol and chemiluminescence reaction of potassium permanganate and formaldehyde in the polyphosphate enhanced by clenbuterol. Clenbuterol in the urine was selectively adsorbed on the clenbuterol-imprinted polymer, which was packed into the flow cell. The formaldehyde and the polyphosphate with potassium permanganate flowed through the flow cell and reacted with the on line adsorbed clenbuterol and produced strong CL. The results show that the sensor was reversible. The CL intensity was linear with clenbuterol concentration from 1.0 × 10⁻⁹ g/mL to 5.0 × 10⁻⁸ g/mL. The detection limit was 3.0 × 10⁻¹⁰ g/mL. The R.S.D. for ng/mL clenbuterol was less than 5% (n = 3). The present method offered a high selectivity and sensitivity that made the quantitative analysis of trace clenbuterol (ng/mL) in the animal urine sample.     

纳米金催化Luminol-AgNO_3化学发光体系测定盐酸阿米替林

碱性条件下,纳米金对Luminol-Ag NO3化学发光体系有增敏作用,盐酸阿米替林对该化学发光体系有显著的增敏作用。基于此,在优化化学发光反应条件的基础上,提出了测定盐酸阿米替林的新方法,并对其化学发光机理进行了探讨。该法测定盐酸阿米替林的线性范围为3.0×10-9~3.0×10-7g/m L,相关系数(r)为0.999 4,检出限(S/N=3)为2.1×10-9g/m L,相对标准偏差(RSD)为2.0%(n=11,ρ盐酸阿米替林=5.0×10-8g/m L)。该法已成功用于药物制剂中盐酸阿米替林含量的测定。     

Determination of Rhein in blood plasma by HPLC with UV detection and its application to the study of bioequivalence

A method is proposed for determining rhein (an active metabolite of diacerein) in human blood plasma by reversed-phase high-performance liquid chromatography with UV detection. The analyte was selectively extracted from blood plasma by liquid-liquid extraction with a 5% solution of tert-butyl methyl ether in ethyl acetate. The recovery of rhein is 68 ± 3%, LOQ 100 ng/mL. The stability of the analytes and linearity, selectivity, sensitivity, reproducibility, and accuracy of the developed method are evaluated. The pharmacokinetics of diacerein in the oral administration of drug formulations by 18 healthy volunteers is studied.     

Determination of proteins at nanogram levels by their quenching effect on the chemiluminscence reaction between luminol and hydrogen peroxide with manganese-tetrasulfonatophthalocyanine as a new catalyst

The manganese-tetrasulfonatophthalocyanine (MnTSPc) catalyzed luminol-hydrogen peroxide chemiluminescence (CL) systems can be quenched in the presence of proteins. A highly sensitive CL quenching method has been developed for the determination of proteins. Under optimum conditions, the linear ranges of the calibration curves were 0.1-20 microg/mL for human serum albumin (HSA), 0.2-20 microg/mL for human gamma-IgG, and 0.5-50 microg/mL for the bovine serum albumin (BSA) with the corresponding detection limits were 1.9 ng/mL, 2.7 ng/mL, and 3.4 ng/mL. The method has been applied to the analysis of total proteins in human serum samples and the results were in good agreement with clinical data provided.     

鲁米诺-AuCl4体系化学发光法测定美洛西林钠

在NaOH介质中, AuCl4-氧化鲁米诺产生化学发光, 美洛西林钠显著增强该体系的发光, 据此建立了一种测定美洛西林钠的流动注射化学发光新方法. 在优化的实验条件下, 该法测定美洛西林钠的线性范围为0.01～30 μg/mL, 检出限为3.0 ng/mL, 对1.0 μg/mL美林钠进行了11次平行测定, 其相对标准偏差为1.0%. 方法已用于生物体液和粉针剂中美洛西林钠的测定.     

化学发光底物分辨双组分免疫分析法测定胶质瘤标志物NSE和CA15-3

本文建立了一种基于辣根过氧化物酶(HRP)和碱性磷酸酯酶(ALP)化学发光底物分辨的双组分免疫分析新技术,用以检测人胶质瘤血清标志物神经元特异性烯醇化酶(NSE)和糖链抗原15-3(CA15-3).实验详细考察了捕获抗体、检测抗体、HRP和ALP酶标记物的用量,结果发现NSE和CA15-3的线性范围分别为0.5～20ng/mL(R20.99)和0.5～20U/mL(R20.99),最低检出限分别为0.2ng/mL和0.2U/mL;高、中和低三个浓度的血清加样回收率良好;天内和天间相对标准偏差均小于10%;且一份血清,两组分同时检测无交叉干扰.综合而言:本法能够一次实验,高灵敏、高特异地同时检测两种疾病标志物,具有血清用量少、检测时间短、操作简单、结果可靠的优点,有望为胶质瘤的临床早期诊断提供坚实的支持.     

Solid Phase Extraction Chemiluminescence Determination of Methamidaphos on Vegetables

IntroductionDuring recent years,organophosphorus pesticides(OPPs)have been widely used in agriculture becauseof their low environmental persistence and high effec-tiveness.However,they have a high acute toxicity.Trace amounts of OPPs may remain in foodstu…