首页 | 本学科首页   官方微博 | 高级检索  
相似文献
 共查询到20条相似文献,搜索用时 15 毫秒
1.
A sensitive and simple chemiluminescent (CL) method for the determination of diclofenac sodium has been developed by combining the flow injection technique and its sensitizing effect on the weak CL reaction between formaldehyde and acidic potassium permanganate. A calibration curve is constructed for diclofenac sodium under optimized experimental parameters over the range 0.040–5.0 µg/mL and the limit of detection is 0.020 µg/mL (3σ). The inter‐assay relative standard deviation for 0.040 µg/mL diclofenac sodium (n = 11) is 2.0%. This method is rapid, sensitive, simple, and shows good selectivity and reproducibility. The proposed method has been successfully applied to the determination of the studied diclofenac sodium in pharmaceutical preparations with satisfactory results. Furthermore, the possible mechanism for the CL reaction has been discussed in detail on the basis of UV and CL spectra. Copyright © 2014 John Wiley & Sons, Ltd.  相似文献   

2.
A simple, rapid and sensitive chemiluminescent (CL) method for the assay of venlafaxine (VEN) in pharmaceutical formulations and serum samples by a two‐chip device is proposed. The method is based on the reaction of this drug with a tris(2,2′‐bipyridyl) ruthenium(II)–peroxydisulphate CL system. The optimum chemical conditions for CL emission were investigated. The calibration graph was linear for the concentration range 0.02–8.0 µg/mL. The detection and quantification limits were found to be 0.006 and 0.018 µg/mL, respectively, while the relative standard deviation (RSD) was <2.0%. The present CL procedure was applied to the determination of VEN in pharmaceutical formulations and serum samples; the recovery levels were in the range 96.5–101.2%. The results suggest that the method is unaffected by the presence of common formulation excipients found in these samples. Copyright © 2012 John Wiley & Sons, Ltd.  相似文献   

3.
Chemiluminescence (CL) detection for the determination of estrogen benzoate, using the reaction of tris(1,10–phenanthroline)ruthenium(II)–Na2SO3–permanganate, is described. This method is based on the CL reaction of estrogen benzoate (EB) with acidic potassium permanganate and tris(1,10–phenanthroline)ruthenium(II). The CL intensity is greatly enhanced when Na2SO3 is added. After optimization of the different experimental parameters, a calibration graph for estrogen benzoate is linear in the range 0.05–10 µg/mL. The 3 s limit of detection is 0.024 µg/mL and the relative standard deviation was 1.3% for 1.0 µg/mL estrogen benzoate (n = 11). This proposed method was successfully applied to commercial injection samples and emulsion cosmetics. The mechanism of CL reaction was also studied. Copyright © 2011 John Wiley & Sons, Ltd.  相似文献   

4.
A new chemiluminescence (CL) method using flow injection has been described for the rapid and sensitive determination of promazine hydrochloride (PMH). The method is based on the CL reaction of PMH with tris(1,10 phenanthroline)ruthenium(II), [Ru(phen)32+] and Ce(IV) in sulfuric acid medium. Effects of chemical variables were investigated employing central composite design and response surface methodology. Under the optimum conditions, the CL intensity was proportional to the concentration of the drug in solution over the ranges 0.020–0.32 and 0.32–32 µg/mL. The limit of detection (signal‐to‐noise ratio = 3) was 0.012 µg/mL. The method was applied successfully to the determination of PMH in drug formulations and human serum (recovery percentages between 96.7 and 105.0%). The relative standard deviation for 11 replicate determinations of 1.5 µg/mL of PMH was 1.7%. The minimum sampling rate was 100 samples per hour. Copyright © 2009 John Wiley & Sons, Ltd.  相似文献   

5.
A simple and rapid capillary electrophoresis (CE) with an acidic potassium permanganate chemiluminescence (CL) detection method was developed to determine three alkaloids (curine, sinomenine and magnoflorine) simultaneously. A laboratory‐built CE–CL detection interface was used. The field‐amplified sample stacking technique was applied to the online concentration of alkaloids. Experimental conditions for CE separation and CL detection were investigated in detail to acquire optimum conditions. Under optimal conditions, the three alkaloids were baseline separated within 6 min, and the detection limits (S/N = 3) ranged from 0.03 µg/mL to 0.49 µg/mL. This method was successfully applied to determine the above three alkaloids in Sinomenium acutum, and the result of the determination of sinomenine was in good agreement with those given by high‐performance liquid chromatography and CE methods. In addition, a possible CL reaction mechanism of sinomenine–KMnO4–H2SO4 was proposed. Copyright © 2013 John Wiley & Sons, Ltd.  相似文献   

6.
Liu Z  Jia F  Wang W  Wang C  Liu Y 《Luminescence》2012,27(4):297-301
A novel method was developed using molecular imprinting technology (MIT) coupled with flow‐injection chemiluminescence (FI‐CL) for highly sensitive detection of phenformin hydrochloride (PH). The phenformin imprinted polymer was synthesized with methacrylic acid (MAA) as a functional monomer and ethylene glycol dimethacrylate (EGDMA) as a cross‐linker. Newly synthesized molecularly imprinted polymer (MIP) particles were packed into a column as a selective recognition element for determination of PH. A CL method for the determination of PH was developed based on the CL reaction of PH with N‐bromosuccinimide sensitized by eosin Y in basic media. The optimization of detection conditions was investigated. The CL intensity responded linearly to the concentration of PH in the range 0.09–2.0 µg/mL, with a correlation coefficient of 0.9920. The detection limit was 0.031 µg/mL. The relative standard deviation for the determination of 1.0 µg/mL PH solution was 1.0% (n = 11). The method was applied to the determination of PH in urine samples, with satisfactory results. Copyright © 2011 John Wiley & Sons, Ltd.  相似文献   

7.
8.
It was found that meloxicam could enhance the chemiluminescence (CL) of the tris(2,2'‐bipyridine) ruthenium(II)–Ce(IV) system in the medium of sulfate acid. Based on this phenomenon a new flow‐injection system with chemiluminescent detection has been proposed for determination of meloxicam. Under optimum conditions, meloxicam had a good linear relationship with the CL intensity in the concentration range of 6.0  10?4 to 1.0 µg/mL and the detection limit was 3.7 × 10?4 µg/mL. The proposed method was applied to detect meloxicam in tablets and a satisfactory recovery was obtained. The possible mechanism for this CL system is also discussed in this paper. Copyright © 2009 John Wiley & Sons, Ltd.  相似文献   

9.
A simple, rapid and sensitive method has been developed for the analysis of fexofenadine (FEX) in pharmaceutical formulations, using a tris(1,10‐phenanthroline)–ruthenium(II) [Ru(phen)32+] peroxydisulphate chemiluminescence (CL) system in a multichip device. Various parameters that influence the CL signal intensity were optimized. These included pH, flow rates and concentration of reagents used. Under optimum conditions, a linear calibration curve in the range 0.05–5.0 µg/mL was obtained. The detection limit was found to be 0.001 µg/mL. The procedure was applied to the analysis of FEX in pharmaceutical products and was found to be free from interference from concomitants usually present in these preparations. Copyright © 2011 John Wiley & Sons, Ltd.  相似文献   

10.
A sensitive and simple chemiluminescent (CL) method for the determination of clomipramine has been developed by combining the flow‐injection analysis (FIA) technique, which is based on the CL intensity generated from the redox reaction of potassium permanganate (KMnO4)–formic acid in sulphuric acid (H2SO4) medium. Under the optimum conditions, the linear range for the determination of clomipramine was 0.04–4 µg/mL, with a correlation coefficient of 0.9988 (n = 10) and a detection limit of 0.008 µg/mL (3σ), and the relative standard deviation (RSD) for 2.0 µg/mL clomipramine (n = 11) is 1.26%. The proposed method has been successfully applied to the determination of the studied clomipramine in pharmaceutical preparations. The possible reaction mechanism is discussed. Copyright © 2011 John Wiley & Sons, Ltd.  相似文献   

11.
Xiong X  Zhang Q  Nan Y  Gu X 《Luminescence》2012,27(5):371-378
A simple one‐step method is established for plasma determination of ibuprofen and its pharmacokinetic study. The method involves simple sample pre‐treatment by dilution, rapid separation by ultrafiltration (UF) and online sensitive detection by chemiluminescence (CL) based on significant intensity enhancement of ibuprofen on the weak CL of potassium permanganate and sodium sulphite in an acidic system. The calibration curve for ibuprofen is linear in the range 0.1–50.0 µg/mL in rat plasma. Average recoveries of ibuprofen at 0.80, 12.0 and 40.0 µg/mL amounted to 98.0 ± 4.2%, 101.2 ± 3.6% and 99.3 ± 5.4%, respectively. Standard deviations of intra‐ and inter‐day measurement precision and accuracy are within ±10.0%. The detection limit for ibuprofen is 10.0 µg/L in plasma samples. Pharmacokinetic study of ibuprofen by the validated method shows that the mean plasma drug concentration–time course confirms to a classical two‐compartment open model with first‐order absorption. The proposed method will be an alternative for pre‐clinical pharmacokinetic study of ibuprofen and other non‐steroidal anti‐inflammatory drugs. Copyright © 2011 John Wiley & Sons, Ltd.  相似文献   

12.
A novel, sensitive and rapid CL method coupled with high‐performance liquid chromatography separation for the determination of carbamazepine is described. The method was based on the fact that carbamazepine could significantly enhance the chemiluminescence of the reaction of cerium sulfate and tris(2,2‐bipyridyl) ruthenium(II) in the presence of acid. The chromatographic separation was performed on a Kromasil® (Sigma‐Aldrich) TM RP‐C18 column (id: 150 mm × 4.6 mm, particle size: 5 µm, pore size: 100 Å) with a mobile phase consisting of methanol–water‐glacial acetic acid (70:29:1, v/v/v) at a flowrate of 1.0 mL/min, the total analysis time was within 650 s. Under optimal conditions, CL intensity was linear for carbamazepine in the range 2.0 × 10?8 ~ 4.0 × 10?5 g/mL, with a detection limit of 6.0 × 10?9 g/mL (S/N = 3) and the relative standard detection was 2.5% for 2.0 × 10?6 g/mL (n = 11). This method was successfully applied to the analysis of carbamazepine in human urine and serum samples. The possible mechanism of the CL reaction is also discussed briefly. Copyright © 2012 John Wiley & Sons, Ltd.  相似文献   

13.
A highly sensitive and simple method for identifying sulpiride in pharmaceutical formulations and biological fluids is presented. The method is based on increased chemiluminescence (CL) intensity of a luminol–H2O2 system in response to the addition of Cr (III) under alkaline conditions. The CL intensity of the luminol–H2O2–Cr (III) system was greatly enhanced by the addition of sulpiride and the CL intensity was proportional to the concentration of sulpiride in a sample solution. Various parameters affecting the CL intensity were systematically investigated and optimized for determination of the sulpiride in a sample. Under the optimum conditions, the CL intensity was proportional to the concentration of sulpiride in the range of 0.068–4.0 µg/mL, with a good correlation coefficient of 0.997. The limit of detection (LOD) and limit of quantification (LOQ) were found to be 8.50 × 10‐6 µg/mL and 2.83 × 10‐5 µg/mL, respectively. The method presented here produced good reproducibility with a relative standard deviation (RSD) of 2.70% (n = 7). The effects of common excipients and metal ions were studied for their interference effect. The method was validated statistically through recovery studies and successfully applied for the determination of sulpiride in pure form, pharmaceutical preparations and spiked human plasma samples. The percentage recoveries were found to range from 99.10 to 100.05% for pure form, 98.12 to 100.18% for pharmaceutical preparations and 97.9 to 101.4% for spiked human plasma. Copyright © 2012 John Wiley & Sons, Ltd.  相似文献   

14.
A new method for the detection of β2 adrenergic agonists was developed based on the chemiluminescence (CL) reaction of β2 adrenergic agonist with potassium ferricyanide–luminol CL. The effect of β2 adrenergic agonists including isoprenaline hydrochloride, salbutamol sulfate, terbutaline sulfate and ractopamine on the CL intensity of potassium ferricyanide–luminol was discovered. Detection of the β2 adrenergic agonist was carried out in a flow system. Using uniform design experimentation, the influence factors of CL were optimized. The optimal experimental conditions were 1 mmol/L of potassium ferricyanide, 10 µmol/L of luminol, 1.2 mmol/L of sodium hydroxide, a flow speed of 2.6 mL/min and a distance of 1.2 cm from ‘Y2’ to the flow cell. The linear ranges and limit of detection were 10–100 and 5 ng/mL for isoprenaline hydrochloride, 20–100 and 5 ng/mL for salbutamol sulfate, 8–200 and 1 ng/mL for terbutaline sulfate, 20–100 and 4 ng/mL for ractopamine, respectively. The proposed method allowed 200 injections/h with excellent repeatability and precision. It was successfully applied to the determination of three β2 adrenergic agonists in commercial pharmaceutical formulations with recoveries in the range of 96.8–98.5%. The possible CL reaction mechanism of potassium ferricyanide–luminol–β2 adrenergic agonist was discussed from the UV/vis spectra. Copyright © 2014 John Wiley & Sons, Ltd.  相似文献   

15.
A novel galangin–potassium permanganate (KMnO4)–polyphosphoric acid (PPA) system was found to have an outstanding response to tryptophan (Trp). Trp determination using this KMnO4–PPA system was enhanced significantly in the presence of galangin. A highly sensitive flow‐injection chemiluminescence (CL) method to determine Trp was developed based on the CL reaction of galangin–KMnO4–Trp in PPA media. The presence of galangin, a member of the flavonol class of flavonoid complexes, greatly increased the luminous intensity of Trp in KMnO4–PPA systems. Under optimized conditions, Trp was determined in the 0.05–10 µg/mL range, with a detection limit (3σ) of 5.0 × 10?3 µg/mL. The relative standard deviation (RSD) was 1.0% for 11 replicate determinations of 1.0 µg/mL Trp. Two synthetic samples were determined selectively with recoveries of 98.4–100.1% in the presence of other amino acids. The possible mechanism is summarized as follows: excited states of Mn(II)* and Mn(III * types are the main means of generating chemical luminescent species, and Trp concentration and luminescence intensity have a linear relationship, which enables quantitative analysis. Copyright © 2014 John Wiley & Sons, Ltd.  相似文献   

16.
A highly sensitive, rapid and economical method for the determination of amlodipine (AM) in biological fluids was developed using a peroxyoxalate chemiluminescence (CL) system in a lab‐on‐a‐chip device. Peroxyoxalate‐CL is an indirect type of CL that allows the detection of native fluorophores or compounds derivatized with fluorescent labels. Here, fluorescamine was reacted with AM, and the derivatization product was used in a bis‐(2,4,6‐trichlorophenyl)oxalate‐CL system. Fluorescamine reacts selectively with aliphatic primary amine at neutral or basic pH. As most of the calcium channel blocker and many cardiovascular drugs do not contain primary amine, the developed method is highly selective. The parameters that influenced the CL signal intensity were studied carefully. These included the chip geometry, pH, concentration of reagents used and flow rates. Moreover, we confirmed our previous observation about the effects of imidazole, which is commonly used in the bis‐(2,4,6‐trichlorophenyl)oxalate‐CL system as a catalyst, and found that the signal was significantly improved when imidazole was absent. Under optimized conditions, a calibration curve was obtained with a linear range (10–100 µg/L). The limit of detection was 3 µg/L, while the limit of quantification was 10 µg/L. Finally the method was applied for the determination of AM in biological fluids successfully. Copyright © 2014 John Wiley & Sons, Ltd.  相似文献   

17.
Measuring low amounts of anti‐erythropoietin antibodies (anti‐EPO Abs) is important to evaluate the therapeutic safety of recombinant human erythropoietin (rhEPO). In this work, a simple, sensitive and high‐throughput chemiluminescent (CL) imaging assay was developed for the detection of anti‐EPO Abs in human sera. The influence of several physicochemical parameters, such as coating conditions, incubation time, detergent concentration and exposure time, were investigated. A calibration curve was established and the range of quantitative detection was 0.12–13.91 ng/mL. The limit of detection (LOD, 3σ) for the CL‐imaging assay was 0.033 ng/mL. Compared to conventional colorimetric enzyme‐linked immunosorbent assay (ELISA), the LOD of the CL‐imaging assay is 50‐fold lower. The recoveries of anti‐EPO Abs in the fortified serum were in the range 87.1–116.9% using the present method, which highlighted the validity of the CL‐imaging assay system to accurately determine the anti‐EPO Abs in serum samples. CL‐imaging assay was used to evaluate the presence of anti‐EPO Abs in serum samples obtained from chronic renal failure (CRF) patients treated with rhEPO. Contrary to what was expected, the sera from CRF patients did not contain anti‐EPO Abs. Copyright © 2008 John Wiley & Sons, Ltd.  相似文献   

18.
An enzyme-linked immunosorbent assay (ELISA) for the Alternaria mycotoxin tenuazonic acid (TeA) was evaluated by comparative analysis of naturally contaminated sorghum grains and sorghum-based infant food, using a stable isotope dilution LC-MS assay (SIDA; limit of detection (LOD) 1.0 μg/kg) as the reference method. LODs of the ELISA were 30 μg/kg in sorghum grains and 220 μg/kg in sorghum-based infant cereals. With SIDA, 100% of the samples (n = 28) had been positive for TeA in a concentration range of 6–584 μg/kg (mean 113 μg/kg). The ELISA consistently detected TeA in all naturally contaminated samples at cut-off levels of 30–60 μg/kg (sorghum) and 200–300 μg/kg (infant cereals), as based on corresponding to SIDA values. Although the ELISA was much less sensitive than the SIDA method, it may be useful as a screening method for sorghum and sorghum-based infant foods and can be employed to identify samples containing elevated concentrations of TeA in food, well below the proposed level of concern (500 μg/kg).  相似文献   

19.
Samples of water, sediments and aquatic weeds were collected from 26 sites in the Nyando River catchment of the Lake Victoria basin in 2005–2006. The objective was to investigate levels of organochlorine pesticides that have either been banned or are restricted for use in Kenya. The pesticides investigated were lindane, aldrin, endosulfan, endrin, dieldrin, DDT, heptachlor and methoxychlor. These pesticides had previously found wide applications in public health and agriculture in Kenya for control of disease vectors and crop pests respectively. Results showed that mean concentrations were highest for methoxychlor (8.817 ± 0.020?µg l?1) in water, sediments (92.893 ± 3.039 µg kg?1), and weeds (39.641 ± 3.045?µg kg?1), the weeds also tended to accumulate aldrin (15.519 ± 3.756?µg kg?1). The results show that the pesticides are still in use and are detected in the catchment. Stringent management and public awareness measures are required to enforce the ban on the organochlorine pesticides in order to safeguard the environment and ecosystems of Lake Victoria.  相似文献   

20.
The occurrence of organochlorine pesticides in the environment has been a major concern, due to their high persistence and the possible impacts of their exposure to humans. Dichlorodiphenyltrichloroethane (DDT) is most hazardous and one of the most widely used organochlorine insecticides. DDT and its main metabolites are highly stable to physical, chemical and biological degradation and are therefore still being detected in many parts of the world. The present study describes dipstick‐based immuno‐chemiluminescence method for the detection of DDT with high sensitivity. Anti‐DDT antibodies raised in chicken (IgY) were used as the biological sensing elements by immobilizing onto nitrocellulose membrane strips in a chemiluminescence (CL)‐based dipstick technique. The photons generated during the biochemical interaction were directly proportional to the DDT concentration. A mean recovery of 81.2–95.6% was obtained for DDT‐spiked fruit juice samples with 2.8–4.6% relative standard deviation (RSD). Using the proposed dipstick‐based immuno‐CL method, DDT was detected with linearity in the range 0.05–1 ng/mL, having a limit of detection (LOD) of 0.05 ng/mL. This method can be used for the rapid, reliable detection of DDT pesticide. Copyright © 2012 John Wiley & Sons, Ltd.  相似文献   

设为首页 | 免责声明 | 关于勤云 | 加入收藏

Copyright©北京勤云科技发展有限公司  京ICP备09084417号