固相萃取—化学发光法测定植物中的吲哚乙酸

植物拟南芥中吲哚乙酸用甲醇超声提取,后经固相萃取小柱净化用化学发光法测定.在多聚磷酸(PPA)介质中,吲哚乙酸对高良姜素-高锰酸钾体系的发光有很强的增敏作用,据此建立了固相萃取-流动注射化学发光测定吲哚乙酸的新方法.在优化条件下,相对化学发光的对数值与吲哚乙酸浓度的对数值在8.0 ×10-9～1.0×10 -7g/mL...     

流动注射化学发光法测定水中的苯胺

基于在多聚磷酸介质中,KMnO4氧化苯胺能产生强化学发光,建立了流动注射化学发光测定苯胺的新方法.在优化条件下,化学发光强度ⅠCL与苯胺的浓度在2.0×10～1.0×10-6 mol/L范围内呈良好的线性关系,回归方程为ⅠCL=63.11 2.37×108c(r=0.9997,n=9),检出限为5.0×10-10 mol/L,对1.0×10-7 mol/L苯胺进行11次测定,其相对标准偏差为0.8%(n=11).已用于环境水体中苯胺的测定,回收率在95.1%～105.1%之间.     

去乙酰毛花苷的流动注射化学发光分析研究

在碱性介质中,去乙酰毛花苷对鲁米诺-KIO4发光体系有明显的抑制作用,且抑制效果与其质量浓度呈良好的线性关系,据此建立了去乙酰毛花苷的流动注射化学发光分析方法。该方法的线性范围为1.0×10-8~1.0×10-5g/mL,检出限为3.1×10-9g/mL,对1.0×10-7g/mL的去乙酰毛花苷进行连续11次平行测定,相对标准偏差为2.3%。可用于相应注射剂分析,并与药典方法进行对照。     

流动注射化学发光法测定头孢氨苄和头孢拉定

基于KMnO4在酸性介质中氧化头孢氨苄和头孢拉定产生微弱的化学发光,同时借助甲醛对发光的增强作用,采用流动注射技术,建立了以上两种头孢类抗生素药物的测定新方法。方法检出限分别为0.096和0.10μg mL;相对标准偏差分别为1.6%和1.8%(n=11),线性范围分别为0.8～25和0.8～32μg mL,进样频率为60次 h。本方法已用于药物制剂的测定。     

Flow-injection chemiluminescence determination of formaldehyde in water

A modification of the Trautz-Schorigin reaction into a flow-injection analysis configuration is described. Different approaches were used at the optimization of chemiluminescence determination of formaldehyde in water based on the reaction of formaldehyde, gallic acid and hydrogen peroxide in an alkaline solution. Detection system with a 218 μl chemiluminescence cell was optimized by both a one-variable-at-a-time method, and a modified simplex method. A calibration graph is linear in the concentration range 4 × 10⁻⁸ to 1 × 10⁻⁵ M HCHO. The detection limit of formaldehyde for a signal-to-noise ratio of 3 is 4 × 10⁻⁸ M. The relative standard deviations for 15 repeated measurements of 1 × 10⁻⁶ and 5 × 10⁻⁶ mol l⁻¹ HCHO are 4.32 and 3.33%, respectively. The analysis time is 1.5 min. The method was applied to the determination of formaldehyde in urban rainwater. A comparison of results found by proposed method with those obtained by fluorimetric reference method provided a good agreement.     

Flow-injection chemiluminescence assay for ultra-trace determination of DNA using rhodamine B-Ce(IV)-DNA ternary system in sulfuric acid media

A novel flow-injection chemiluminescence method for the determination of DNA at ultra-trace level has been established. In 0.8 M sulfuric acid media, the chemiluminescence of the rhodamine B-cerium (IV) or Ce(IV) system is enhanced by DNA, activated previously by imidazole-HCl buffer solution (pH 7.0). The enhanced intensity of chemiluminescence is in proportion to log DNA concentration 1.0×10⁻⁸ to 0.1 μg ml⁻¹ for herring sperm DNA and 2.0×10⁻⁶ to 0.2 μg ml⁻¹ for calf thymus DNA with 3σ detection limits of 8.3×10⁻⁹ μg ml⁻¹ for herring sperm DNA and 3.5×10⁻⁷ μg ml⁻¹ for calf thymus DNA, respectively. The relative standard deviation for 1.0×10⁻⁴ μg ml⁻¹ herring sperm DNA was 0.99% and 2.0×10⁻³ μg ml⁻¹ for calf thymus DNA was 1.1% (n=11). Using the optimized system, DNA contents in six synthetic samples has been determined with recoveries of 99.5-109.0%. The possible mechanism has also been studied in this paper.     

Flow-injection chemiluminescence determination of fluoroquinolones by enhancement of weak chemiluminescence from peroxynitrous acid

A flow-injection chemiluminescence (CL) method is described for the determination of fluoroquinolones including ciprofloxacin, norfloxacin and ofloxacin. The method is based on the enhancement by these compounds of the weak CL from peroxynitrous acid. The linear ranges are 1.0×10⁻⁷ to 1.0×10⁻⁵ mol l⁻¹ for ciprofloxacin and norfloxacin, and 3.0×10⁻⁷ to 3.0×10⁻⁵ mol l⁻¹ for ofloxacin, respectively. The detection limits (S/N=3) are 4.5×10⁻⁸ mol l⁻¹ ciprofloxacin, 5.9×10⁻⁸ mol l⁻¹ norfloxacin and 1.1×10⁻⁷ mol l⁻¹ ofloxacin, respectively. The proposed method was applied to the determination of fluoroquinolones in pharmaceutical preparations.     

KMnO4-乙二醛化学发光法测定苦味酸

基于苦味酸对KMnO4-乙二醛化学发光体系的抑制作用,建立了苦味酸的流动注射化学发光测定方法;在最佳条件下,方法对苦味酸的检出限为1.0×10 -12 mol/L,线性范围为1.0×10-11～1.0×10 -3 mol/L;对1.0×10-7 mol/L苦味酸平行测定11次,其RSD为2.5％.该方法可应用于水样中的...     

流动注射化学发光分析法测定利福平

在酸性条件下,KMnO4能氧化利福平产生弱化学发光,并且,利福平能极大的增敏Na2SO3-KMnO4体系的化学发光信号。基于此,结合流动注射技术,建立了测定利福平的新方法。在优化的条件下,利福平在5.0×10-8g/mL~1.0×10-5g/mL范围内与化学发光强度呈良好的线性关系,检出限为3×10-8g/mL。对2.0×10-6g/mL的利福平进行11次平行测定,相对标准偏差为2.6%。该法用于胶囊和滴眼液中利福平的测定,并初步探讨了该化学发光反应机理。     

Flow-injection chemiluminescence determination of tetracyclines with in situ electrogenerated bromine as the oxidant

By designing a novel flow-through electrolytic cell (FEC), bromine was produced near to the surface of the platinum electrode by electrochemical oxidation of acidic KBr. The fast and weak chemiluminescence signal produced by the chemical reaction of the electrogenerated bromine with H₂O₂ was greatly enhanced by tetracyclines Based on these observations, a new, sensitive and simple electrogenerated chemiluminescence (ECL) method for the determination of tetracyclines was developed. Under the optimum experimental conditions, the calibration graphs are linear over the range 3.0×10⁻⁸ to 5.0×10⁻⁵ g ml⁻¹ for tetracycline, 2.0×10⁻⁷ to 2.4×10⁻⁵ g ml⁻¹ for oxytetracycline and 1.0×10⁻⁷ to 5.0×10⁻⁵ g ml⁻¹ for chlortetracycline. The limits of detection (S/N=3) are 1.0×10⁻⁸ g ml⁻¹ for tetracycline, 7.0×10⁻⁸ g ml⁻¹ for oxytetracycline and 1.5×10⁻⁷ g ml⁻¹ for chlortetracycline. For the determination 5.0×10⁻⁷ g ml⁻¹ tetracycline, the relative standard deviation was <5%. The proposed method was used to determine tetracyclines in pharmaceutical formulations.     

Flow-injection chemiluminescence determination of chloroquine using peroxynitrous acid as oxidant

A new flow-injection chemiluminescence (CL) method for determination of chloroquine is proposed based on a stronger chemiluminescence of chloroquine in hydrogen peroxide-nitrite-sulfuric acid medium. The proposed method allows the measurement of chloroquine over the range of 3.0×10⁻⁷ to 1.0×10⁻⁵ mol l⁻¹. The detection limit is 8.6×10⁻⁸ mol l⁻¹, and the relative standard deviation for 1.0×10⁻⁶ mol l⁻¹ chloroquine (n=11) is 1.6%. The CL mechanism is also discussed.     

化学发光法测定水杨酸

根据在硫酸酸性溶液中高锰酸钾能氧化水杨酸产生化学发光反应 ,而乙二醛的存在可使发光强度增强 ,建立了一种测定水杨酸的化学发光分析法 ,检出限为 8.0× 1 0 -6mol/L,线性范围为 4.0× 1 0 -3～ 6.0× 1 0 -5mol/L。该法巳用于样品复方苯甲酸醇溶液中水杨酸的测定。     

流动注射化学发光法测定盐酸普萘洛尔

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。     

流动注射化学发光法测定氯化血红素

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。     

Flow-injection chemiluminescence determination of aminomethylbenzoic acid and aminophylline based on N-bromosuccinimide-luminol reaction

A novel and sensitive chemiluminescence (CL) method for the determination of aminomethylbenzoic acid and aminophylline coupled with flow-injection analysis (FIA) technique is developed in this paper. It is based on the inhibition effect of the studied drugs on the chemiluminescence emission of N-bromosuccinimide-luminol (NBS-luminol) system. Under the optimum conditions, the decreased CL intensity is linear with the concentration of aminomethylbenzoic acid in the range of 2×10⁻⁸ to 1.0×10⁻⁶ g ml⁻¹ and with the concentration of aminophylline in the range of 1×10⁻⁷ to 7.0×10⁻⁶ g ml⁻¹, respectively. The detection limit is 7.0×10⁻⁹ g ml⁻¹ for aminomethylbenzoic acid (3σ) and 3.4×10⁻⁸ g ml⁻¹ for aminophylline (3σ). The relative standard deviations (R.S.D.) for 11 parallel measurements of 2.0×10⁻⁷ g ml⁻¹ aminomethylbenzoic acid and 1.0×10⁻⁶ g ml⁻¹ aminophylline are 2.6 and 3.0%, respectively. The proposed methods have been applied for the determination of the studied drugs in their pharmaceutical formulations with satisfactory results. The possible use of the proposed system for the determination of aminomethylbenzoic acid in plasma sample was also tested. The possible inhibition mechanism of aminomethylbenzoic acid and aminophylline on luminol-NBS system was discussed briefly.     

Flow-injection chemiluminescence determination of epinephrine in pharmaceutical preparations using raw apple juice as enzyme source

Raw apple juice exhibits the activity of polyphenol oxidase which can be employed for the determination of mono-, di- and polyhydric phenols. The chemiluminescence detection in the two-channel manifold was used to develop the new procedure for determination of epinephrine. Epinephrine can be determined by this method in pharmaceutical preparations in concentration ranges 1.0–10.0 and 10.0–25.0 mg l⁻¹, with a detection limit of 0.2 mg l⁻¹. Good selectivity against typical antioxidants and other coexisting substances was achieved. Relatively slow loss of the enzyme activity was observed during 1 week. The proposed method is very simple. Fresh juice solution from one apple can be prepared in 10 min and used for at least 8 h with excellent precision. Consumption of luminol solution was 0.15 ml min⁻¹. The throughput was 20 samples per hour.     

KMnO4-乙二醛化学发光体系测定5-磺基水杨酸的流动注射分析

酸性介质下,KMnO4可以氧化5-磺基水杨酸产生化学发光,乙二醛对该体系有增敏作用。结合流动注射技术,建立了测定5-磺基水杨酸的流动注射化学发光方法。方法线性范围为2.0×10-8～2.0×10-5mol/L,检出限为2.0×10-9mol/L,对2.0×10-6 mol/L的5-磺基水杨酸平行测定11次,相对标准偏差为1.9%。该法可用于强力霉素废水中5-磺基水杨酸的测定。     

化学发光法同时测定色氨酸和半胱氨酸的研究

基于色氨酸和半胱氨酸对Ru(pheo)32 -Ce(Ⅳ)体系化学发光的增强作用及其发光动力学性质的显著差别,提出了一种化学发光法同时测定这两种氨基酸的新方法.在优化的实验条件下,该方法测定色氨酸和半胱氨酸的线性范围分别为0.05～2.0 μg/mL和0.05～3.0 μg/mL,检出限分别为0.03 μg/mL和0.02 μg/mL.将其应用于合成样品中两种氨基酸的同时测定.结合文献提出了可能的化学发光反应机理.     

流动注射化学发光法测定兽药制剂中沙拉沙星

基于沙拉沙星对Ag(III)络合物-H2SO4体系化学发光信号的增敏作用,提出了一种流动注射-化学发光测定沙拉沙星的新方法。考察和优化了影响化学发光强度的条件。沙拉沙星在2.0×10-7～1.0×10-5g/mL范围内,其校准曲线具有良好的线性。方法的检出限为1.2×10-7g/mL,相对标准偏差0.5%～1.2%。该方法已用于沙拉沙星兽药制剂的质量检测,回收率为83.3%～96.3%。通过比较其荧光光谱和化学发光光谱,讨论了该体系的化学发光机理。     

Determination of fenfluramine based on potassium permanganate-calcein chemiluminescence system

Calcein was found to be able to use as chemiluminescence reagent and post-chemiluminescence was observed when fenfluramine was injected into the mixture after the CL reaction of calcein–potassium permanganate. Based on this phenomenon, a flow injection CL method was established for the determination of fenfluramine. The possible CL mechanism was proposed. The CL intensity was correlated linearly with the concentration of fenfluramine over the range of 1.0 × 10⁻⁷ to 6.0 × 10⁻⁶ g mL⁻¹ and the detection limit was 6 × 10⁻⁸ g mL⁻¹. The relative standard deviation was 2.2% for 5.0 × 10⁻⁷ g mL⁻¹ fenfluramine (n = 11). This method was applied to the determination of fenfluramine in weight-reducing tonic successfully.