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Carmen Gómez-Benito Sagrario Torres-Cartas 《International journal of environmental analytical chemistry》2013,93(2):152-165
In this work, a sensitive flow injection chemiluminescence (FI-CL) method for the determination of nematicide Fenamiphos in a rapid and simple way is proposed. Fenamiphos is first photodegraded in basic medium. These photofragments react with Ce(IV) providing the chemiluminescence signal. To the authors’ knowledge, no chemiluminescence method has been described in the literature for the determination of the nematicide Fenamiphos. All physical and chemical parameters in the flow injection chemiluminescence system were optimized in order to obtain the best sensitivity, selectivity and sample throughput. Before the injection of the sample in the FI-CL system, a preconcentration step with solid phase extraction C18 cartridges was performed. By applying solid phase extraction (SPE) to 250?mL of standard (final volume 10?mL), the linear dynamic range was between 3.4 and 60?µg?L?1, and the detection limit was 1?µg?L?1. When SPE was applied to 500?mL of standard (final volume 10?mL), the detection limit was 0.5?µg?L?1. These detection limits are below the emission limit value established by the Spanish Regulations of the Hydraulic Public Domain for pesticides (50?µg?L?1) and of the same order as the limit established for total pesticides (0.5?µg?L?1) at European Directive on the quality of water for human consumption. The sample throughput was 126 hour?1. Intraday and interday coefficients of variation were below 10% in all cases. No interference was registered in presence of usual concentrations of anions, cations and other organophosphorus pesticides. The method was successfully applied to the analysis of environmental water samples, obtaining recoveries between 96 and 107.5%. 相似文献
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A simple chemiluminometric method using flow injection has been developed for the determination of paracetamol (acetaminophen), based on the chemiluminescence produced by the reduction of tris(2,2′-bipyridyl)ruthenium(III). The latter is obtained by oxidation of tris(2,2′-bipyridyl)ruthenium(II) by potassium permanganate in dilute sulphuric acid in the presence of paracetamol. A standard or sample solution was injected into the ruthenium(II) stream (flow rate 1.5 ml min−1) which was then merged with potassium permanganate in dilute sulphuric acid stream (flow rate 0.5 ml min−1). The chemiluminescence intensity is enhanced by the presence of manganese(II) ions. Under the optimum conditions, a linear calibration graph was obtained over the range of 0.3-50.0 μg ml−1 and the detection limit was 0.2 μg ml−1 (s/n = 3). The relative standard deviation of the proposed method calculated from 20 replicate injections of 5.0 μg ml−1 paracetamol was 1.1%. The sample throughput was 90 h−1. The method was successfully applied to the determination of paracetamol in commercial pharmaceutical formulations. 相似文献
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S. M. Sultan Aladdin M. Almuaibed A. Townshend 《Fresenius' Journal of Analytical Chemistry》1998,362(1):167-169
A new flow injection chemiluminescence method for the assay of medazepam is explored. The method involves the use of permanganate
in sulfuric acid for the oxidation of medazepam with the emission of chemiluminescence detected by a photomultiplier tube.
A simplex procedure was employed for optimising the conditions for high sensitivity detection, which were found to be 1.03
× 10–3 mol L–1 permanganate, 0.153 mol L–1 sulfuric acid and 3.43 mL min–1 flow rate. The linear calibration range was 3.7 × 10–5 to 1.7 × 10–3 mol L–1. The detection limit (3σ) and the sample throughput were 1.85 × 10–5 mol L–1 and 100 per hour, respectively. The relative standard deviation for 5 replicate determinations of 1.9 × 10–4 mol L–1 medazepam was 0.15%. Common excipients (starch, glucose, maltose, lactose) used in pharmaceutical preparations had no effect.
Received: 2 February 1998 / Revised: 20 May 1998 / Accepted: 25 May 1998 相似文献
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流动注射化学发光法测定氯化血红素 总被引:2,自引:0,他引:2
在甲醛存在的条件下,在酸性溶液中KMnO4与氯化血红素能够发生化学发光反应,产生很强的化学发光。据此采用流动注射技术,建立了一种利用KMnO4-甲醛-氯化血红素化学发光体系测定氯化血红素的化学发光分析法。方法的检出限为6×10-8g/mL;相对标准偏差为1.8%(2.0×10-6g/mL氯化血红素,n=11);线性范围为2.0×10-7~8.0×10-6g/mL。本法用于新鲜鸡血中氯化血红素的测定,结果与标准方法测得值一致。并对化学发光反应的机理进行了探讨。 相似文献
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流动注射化学发光法测定盐酸普萘洛尔 总被引:2,自引:0,他引:2
在酸性条件下,KMnO4氧化盐酸普萘洛尔可产生化学发光,Fe2 的存在对于这一化学发光反应具有增敏作用,基于此建立了测定盐酸普萘洛尔的化学发光分析法。在选定的实验条件下,盐酸普萘洛尔的质量浓度在4.0×10-7~1.0×10-5g mL范围内与化学发光强度具有线性关系(相关系数为0.9992),检出限为1×10-7g mL盐酸普萘洛尔,相对标准偏差为2.9%(4.0×10-6g mL盐酸普萘洛尔,n=11)。该法已用于盐酸普萘洛尔片剂中盐酸普萘洛尔的测定,并与药典方法进行了对照。 相似文献
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流动注射-化学发光法测定头孢拉定 总被引:13,自引:0,他引:13
1 引 言头孢拉定 (cephradine ,CEP)是广泛用于临床治疗的一种头孢类抗生素药物。目前对其测定的主要方法有高效液相色谱法、分光光度计、荧光法和吸附极谱法等。利用Ce 与某些含巯基的化合物作用产生化学发光从而测定这些化合物的研究已有文献报道 ,但未见用于头孢拉定的测定。头孢拉定的降解产物含有巯基 ,本文采用流动注射技术考察了该降解产物与Ce 作用产生化学发光的条件 ,发现罗丹明 6G对该化学发光体系有很强的增敏作用 ,据此建立了测定头孢拉定的新方法。该方法用于胶囊中头孢拉定含量的测定 ,结果令人满意… 相似文献
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Flow injection electrogenerated chemiluminescence determination of vanadium and its application to environmental water sample 总被引:1,自引:0,他引:1
A selective flow injection electrogenerated chemiluminescence(CL) method for the determination of vanadium is described in this paper. It was based on the chemiluminescence reaction of luminol with vanadium(II), which was on-line electrogenerated from vanadate using a flow-through carbon electrolytic cell. Under the optimal conditions, the CL intensity was linear to the concentration of vanadium in the range of 5.0x10(-10)-1.0x10(-7) gml(-1) with a detection limit of 2x10(-10) gml(-1) vanadium. The relative standard deviation was 4% for 5.0x10(-8) gml(-1) vanadium in 11 repeated measurements. The method has been successfully applied to the determination of vanadium in environmental water samples. 相似文献