微量硼的荧光光度测定法

本文拟定了一个用荧光法测定微量硼的新方法,其线性范围为0～40μg/ml,检测下限为0.04μg/ml。用此方法测定了钢样及高温铁基镍合金中的微量硼,结果令人满意。     

荧光比色法测定人血白蛋白注射液中利凡诺的残留量

根据利凡诺在特定波长下,其水溶液呈黄绿色荧光这一特点,我们制定了荧光比色法测定人血白蛋白注射液中利凡诺残留量的方法。实验结果证明,本法特异性强、灵敏度高、重复性好并操作简便、快速、准确,便于应用。     

Derivatization of Xanthomegnin for Fluorometric Determination

Abstract

A derivatization procedure was developed for the fluorometric determination of purified xanthomegnin. A highly fluorescent product is formed by reaction of xanthomegnin with ammonia and hydrogen peroxide under defined conditions. The derivative is a light brown compound that can easily be dissolved in water or polar organic solvents. Its excitation and emission wavelengths in methanol are 340 and 445 nm, respectively. As little as 0.1 ng of xanthomegnin can be detected using high pressure liquid chromatography in a reverse phase system with fluorescence detection.     

葡萄糖氧化酶催化荧光测定的非酶体系研究

多数氧化酶及其底物都是重要的临床检验指标[1]，目前普遍采用酶荧光法或酶显色法，通过氧化酶催化氧化底物生成H刃。，过氧化物酶（HRP）催化H刃2氧化生成荧光／生色底物，实现间接测定［’j．酶法测定的缺点是体系不稳定、反应条件苛刻、费用较高．最近Mitani等［’j报道了非酶法化学发光测定葡萄糖氧化酶，灵敏度高，但需要特殊试剂，且测定时间较长．我们用Fenton反应［‘j将H。O。转化为羟基自由基（“OH），进而氧化对苯二甲酸生成荧光物质，建立了荧光测定葡萄糖氧化酶的非酶法，详细研究了荧光指示剂的选择、Fenton试剂的改进…     

镁—8羟基喹啉—5—磺酸荧光法测定血清镁浓度

血清中的镁离子与8-羟基喹啉-5-磺酸的络合物在碱性条件下可产生黄绿色荧光(Ex370 nm,E_M500 nm),当血清镁浓度在0.04～2.5μg/ml范围内与荧光强度直线相关(r=0.9996);平均回收率为99.765=3.51(SD)％,相对标准偏差为3.52％(n=21)。方法简便灵敏,为监测血清镁浓度及镁离子药物动力学研究提供了可行方法。     

2,3—二氨基萘荧光光度法测定湘泉酒所用水源中的硒

在ｐＨ１．５－２．０酸性溶液中２，３－二氨基萘选择性与四价硒离子反应，生成４，５－苯并基硒脑绿色荧光物质，用环已烷萃取，其荧光强度与Ｓｅ＾４＋的含量成正比，可定量测定硒的含量。     

磷、砷、硅钼杂多酸-罗丹明6G荧光猝灭法连续测定磷、砷、硅的研究

本文报道了在非离子表面活性剂PVA存在下,磷、硅、砷钼杂多酸-罗丹明6G形成离子缔合物,使罗丹明6G荧光猝灭。研究了罗丹明6G-磷、砷、硅钼杂多酸体系荧光光谱,形成条件和配合物组成。试验了共存离子的干扰。应用此方法对铜合金中磷、砷、硅进行同时测定,结果满意。     

荧光法测定水样中的硒(Ⅳ)、硒(Ⅵ)和有机硒

本文提出了水样中硒（Ⅳ）、硒（Ⅵ）和有机硒的荧光测定方法。基于酸性介质中２,３－二氨基萘与硒（Ⅳ）的选择性反应,直接测定硒（Ⅳ）;利用盐酸还原硒（Ⅵ）和ＨＮＯ３－ＨＣｌＯ４消化有机硒后,用差减法分别测出硒（Ⅵ）和有机硒。检出限０．０７μｇ／Ｌ,线性范围０～１０μｇ／Ｌ。硒（Ⅳ）、硒（Ⅵ）和有机硒的相对标准偏差与回收率分别为２．４％和９８．５％～１０１．５％、３．１％和９４．８％～１０３％、４．０％和９４．５％～９８．８％。     

Sodium Coumarin 6-Sulfonate,A Fluorometric Ion-Pairing Reagent for Tertiary Amines. Application to the Determination of Chlorpheniramine Maleate

Abstract

A study of sodium coumarin 6-sulfonate as a fluorescent ionpair reagent indicated that it could be useful in the analysis of tertiary amines such as chlorpheniramine maleate. The physical properties of the coumarin sulfonate that make it suitable as a fluorescent ion-pair reagent for basic drugs are its high relative quantum yield (0.76) and its acidity (pKa of ?7.66). Methylene chloride containing 5% n?pentanol was used to extract the coumarinchlorpheniramine ion-pair from aqueous solution. It was found that a 10^?2 M coumarin concentration yielded a 92% recovery of chlorpheniramine at pH 5. Following phase separation, the coumarin species was completely ionized by the addition of tetrabuty1 ammonium hydroxide to the organic phase. After irradiation for 30 min using long wavelength ultraviolet light (365 nm), the fluorescence intensity of the sample was measured using excitation and emission wavelengths of 400 and 540 nm, respectively. Comparison of fluorescence data of spiked aqueous samples to that of a chlorpheniramine maleate standard curve performed concurrently gave drug concentration in the samples. The calibration curve was linear in the 50–1000 ng/ml range (0.13 ? 2.6 × 10 ^?6 M). The procedure allowed the determination of chlorpheniramine maleate with an accuracy of 4–6% and a precision of 2–6% RSD (relative standard deviation). The minimum detectable concentration of drug (S/N = 2) that can be assayed by this method is 50 ng/ml of the maleate salt (35.3 ng/ml of chlorpheniramine free base).     

Colorimetric Determination of Propofol in Bulk form,Dosage Form and Biological Fluids

ABSTRACT

Propofol is coupled with 2, 6-dichloroquinone-4-chlorimide (DCQ) in a reaction buffered at pH 9.6 to give a colored product having an analytically useful maximum at 635 nm. The factors affecting the color generation were optimized and incorporated in the procedure. The reacted propofol has a molar absorptivity of 3.9 × 10^?4 L mol^?1 cm^?1, and Beer's law is obeyed for concentrations 1-5 μg ml^?1 with detection limit 0.25 μg ml^?1. The method was found applicable to biological fluids (plasma and urine) spiked with propofol at concentration levels 1-5 μg ml^?1 for plasma and 1-5 μg 0.5 ml^?1 urine (less sensitivity is obtained with urine volumes above 0.5 ml) with detection limits 0.28 μg ml^?1 for plasma and 0.4 μg 0.5 ml^?1 urine. The average recovery for the commercial preparation (1% w/v propofol emulsion intravenous injection for infusion) was 99.54% with an RSD of 1.05%. The method was validated by an adopted HPLC method. The results obtained by the HPLC method for the commercial preparation were statistically compared with the proposed method and evaluated at the 95% confidence limits.     

荧光法测定碱性磷酸酶及其标记物

本文研究了以４－甲基伞形酮磷酸酯（４－ＭＵＰ）为底物测定碱性磷酸酶（ＡＬＰ）活性的高灵敏荧光法及其应用于人血清ＩｇＧ的含量测定。通过纯化４－ＭＵＰ，优化分析条件，使方法的灵敏度有较大提高，实用性也得到改善，测定ＡＬＰ的线性范围为１．７×１０＾－５￣１．７×１０＾－８ＩＵ／ｍＬ，检出限为４．０×１０＾－９ＩＵ／ｍＬ，本法已成功地应用于血清样品ＡＬＰ的测定。作为一个例子，通过测定免疫标记物ＨｕＩｇＧ－     

Polarographic Determination of Lisinopril in Pharmaceuticals and Biological Fluids Through Treatment with Nitrous Acid

 A simple and highly sensitive polarographic method was developed for the determination of lisinopril in dosage forms and biological fluids. The method is based on treatment of the compound with nitrous acid followed by measuring the cathodic current produced by the resulting nitroso derivative. The polarographic behavior was studied adopting direct current (DC_t), differential pulse (DP) and alternating current (AC_t) polarography. A well-defined, diffusion-controlled cathodic wave over the pH range of 1.0–8.0 was obtained in Britton-Robinson buffers (BRb). At pH 3.0, the value of limiting diffusion-current constant (K) was 8.42 ± 0.23 (n = 7). The limiting diffusion current-concentration relationship was found to be rectilinear over the range of 2–24 μg/mL and 0.1–20 μg/mL using DC_t and DP polarographic modes, respectively. The minimum detectability was (S/N = 2) 0.02 μg/mL (4.54 × 10⁻⁸ M). The proposed method was successfully applied to the determination of lisinopril either per se or in dosage forms and the results obtained were in good agreement with those given using a reference method. The proposed method was further applied to the determination of lisinopril in spiked human urine and plasma. The percentage recoveries adopting the DP polarographic mode were 99.71 ± 1.87 and 97.16 ± 1.09, respectively. Received October 18, 2001; accepted July 31, 2002     

Fluorometric determination of urea in alcoholic beverages by using an acid urease column-FIA system

An acid urease column was applied to a fluorometric flow-injection analysis (FIA) system as a recognition element for determination of urea in rice wines.

The acid urease has specific properties of showing its catalytic activity in low pH range and tolerance to ethanol in comparison to those of a urease from jack-beans. The enzymes were covalently immobilized onto porous glass beads with controlled pore size and then, packed into a small polymer column. The flow-type of the biosensing system was assembled with a sample injection valve, the immobilized enzyme column, and a flow-through quartz cell attached to a fluorescent spectrophotometer. Citrate buffer (50 mM, pH 5.0) as the carrier solution was continuously pumped through the system. Sample solutions were introduced into the system via a rotary injection valve. A standard urea solution was measured through monitoring variations in fluorescent intensity attributable to fluorescent isoindole derivatives formed by coupling with ammonia molecules released in the enzymatic hydrolysis of urea and orthophthalaldehyde reagents. The fluorescent intensity was measured under the conditions of λ_ex = 415 nm and λ_em = 485 nm. A wide, linear relationship was obtained between the concentration of urea (1.0–100 μM) and the variation in fluorescent intensity. The monitoring did not suffer from ethanol and various amino acids contained in rice wines. Real samples pretreated with ion exchange resins for removal of endogenous ammonia were introduced into the FIA system and urea in the samples was determined. These results were compared with those obtained with use of an F-kit method. The proposed FIA system should present sensitive, selective and convenient analysis of urea in alcoholic beverages.     

Simultaneous Determination of Acetaminophen with Orphenadrine Citrate,Ibuprofen or Chlorzoxazone in Combined Dosage Forms by Zero-Crossing Derivative Spectrophotometry

Abstract

A derivative spectrophotmetric procedure for the simultaneous determination of acetaminophen-orphenadrine citrate, acetaminophen-ibuprofen and acetaminophen-chlorzoxazone, binary mixtures is described. The procedure minimises the mutual interference between these drugs in mixtures and allows the determination of these compounds without a previous extraction step. The precision of the method, expressed as the relative standard deviation, is better than 4%. The method has been successfully applied to laboratory mixtures and commercial tablets containing these drugs.     

过氧化氢酶荧光分析法及其在海洋水生生物酶活力测定中的应用

建立了一种简便、灵敏的测定过氧化氢酶的方法.方法的线性范围为1.7×10^-3～1.7×10^-2U/mL,检测限(LD=3S₀/S)为8.5×10^-4U/mL.将其用于海洋生物样品中过氧化氢酶活力的测定,结果令人满意.     

槲皮素荧光光度测定法的研究

本详细研究了表面活性剂十二烷基磺酸钠存在下，槲皮素与锆形成三元荧光光胶束配的条件，并建立了测定槲皮素的荧光光度法。在０．９ｍｏｌ／Ｌ盐酸介质中，槲皮素与锆（Ⅳ），ＳＬＳ形成１：４：４的黄绿色荧光配合物，激发波长４３２。１ｎｍ，发射波长５０１。３ｎｍ，线性范围为０．３０×１０－６－１．１１×１０－５ｍｏｌ／Ｌ，检测限为３．７９×１０－７ｍｏｌ／ Ｌ。所拟方法用于芦丁酸水解产物的测定及槐花中回收率的     

Fluorometric Determination of Cellulase

Abstract

A fluorometric procedure is described for the determination of the enzyme cellulase. The method is based upon the hydrolysis of the nonfluorescent substrate, resorufin acetate, by the enzyme to give the highly fluorescent resorufin (λ_ex = 540 mμ;, λ_em = 580 mμ). By this procedure from 0.00010 to 0.060 units per ml. of cellulase can be determined with an accuracy and deviation of about 1.5%. Evidence is offered to demonstrate cellulase, and not esterase, activity.