流动注射化学发光测定尿液和血清中痕量安乃近

目的:建立快速测定痕量安乃近的新方法。方法:本文以安乃近在一定浓度范围内与氨基苯二酰一肼-K3Fe(CN)6化学发光降低值的线性关系为基础,采用抑制化学发光法设计出一种流动注射流路,建立了一种快速、灵敏测定安乃近的方法。结果:测定的线性范围为0.1～100 ng·mL～1,检出限为0.03 ng·mL～1,RSD小于2.8％。该方法成功的监测了口服安乃近后10 h内人体尿液中安乃近含量,结果表明安乃近排出率为11.42％。结论:该方法简便快速,灵敏度高,选择性好。     

流动注射化学发光法测定人尿液中尿酸的含量

目的:建立一种快速、灵敏地测定人尿液中尿酸(UA)含量的新方法。方法:利用在碱性条件下,UA可以选择性地猝灭抗坏血酸与荧光素-表面活性剂-铜离子混合物产生的化学发光,结合流动注射技术,建立了流动注射化学发光法直接测定人尿液中UA含量的方法。反应试剂的浓度分别为氢氧化钠溶液0.5mol/L、荧光素5.0×10-4mol/L、铜离子1.0×10-4mol/L、溴化十六烷基三甲铵(CTMAB)5.0×10-3mol/L、抗坏血酸25mg/L,主泵(P1)、副泵(P2)流速均为2.5ml/min,光电倍增管负高压为800V。结果:UA的检测质量浓度在0.1²0mg/L范围内线性关系良好(r=0.999 0),检出限为3.3×10-2mg/L,平均加样回收率为99.63%,精密度RSD为1.2%(n=11)。结论:本方法操作简便、灵敏度高、选择性好,为尿液中UA含量测定提供了一种新方法。     

流动注射化学发光法测定人尿液中纳克水平乙酰螺旋霉素

目的建立流动注射抑制化学发光测定乙酰螺旋霉素的新方法。方法在碱性介质中乙酰螺旋霉素能强烈抑制luminol-K₃Fe(CN)6化学发光反应。本文以乙酰螺旋霉素在一定浓度范围内与luminol-K₃Fe(CN)6化学发光强度降低值的呈线性关系为基础,结合流动注射技术,快速测定乙酰螺旋霉素。结果测定的线性范围为0.1～100 μg·L^-1,检测限为40 ng·L^-1(3σ),RSD小于3.0%(n=8)。结论该法简便快速、灵敏度高、选择性好,可用于药物、人血清中的乙酰螺旋霉素含量的测定,监测口服乙酰螺旋霉素后人尿液中乙酰螺旋霉素的排泄状况。     

流动注射化学发光法测定左炔诺孕酮含量

目的建立药品中左炔诺孕酮含量测定的方法.方法流动注射化学发光法.结果左炔诺孕酮在0.01～1 mg·L-1范围内呈良好线性关系,r=0.999 7,对0.1 mg·L-1的左炔诺孕酮连续平行测定11次,其相对标准偏差为2.4%,该法的检出限为5.4 μg·L-1L(3σ).结论该方法灵敏度高,线性范围宽,已成功测定了片剂中左炔诺孕酮含量,结果令人满意.     

流动注射化学发光法测定氨苄西林钠的含量

目的建立测定氨苄西林钠新方法。方法在氢氧化钠介质中,高碘酸钾氧化鲁米诺产生化学发光,氨苄西林钠显著增强该体系的发光,据此建立了一种简单、快速测定氨苄西林钠的流动注射化学发光新方法。结果在优化的试验条件下,线性范围为0.01～10μg/ml,检出限(3δ)为3.0ng/ml,对1μg/ml氨苄西林钠进行了11次平行测定,其相对标准偏差为1.4%。结论将本法用于粉针剂中氨苄西林钠的测定,结果令人满意。     

流动注射-抑制化学发光法测定雷尼替丁

目的:建立雷尼替丁含量测定的流动注射化学发光新方法。方法:基于在弱碱性的多聚磷酸钠介质中,雷尼替丁对二价铜离子-过氧化氢-罗丹明B化学发光体系具有强烈的抑制作用而建立的一种新的流动注射化学发光分析法。结果:发光信号的降低值(ΔI)与雷尼替丁的质量浓度在5．0～1000μg·L~(-1)范围内呈良好的线性关系,平均回收率为98．9%～102．9%。对100μg·L~(-1)的雷尼替丁连续进行11次平行测定,其相对标准偏差为3．0%。根据IUPAC建议,计算其检出限为2．7μg·L~(-1)(3σ)。结论:该法可用于胶囊中雷尼替丁含量的测定。     

流动注射化学发光法测定溶菌酶含量

目的建立测定溶菌酶的流动注射化学发光法。方法在酸性介质中,高锰酸钾能氧化溶菌酶产生化学发光,而甲醛能够显著增强该体系的发光强度。据此建立简单快速测定溶菌酶的流动注射化学发光法。结果在最优条件下,溶菌酶的线性范围在0.05~0.34 mg/mL之间,检测限是7.15μg/mL。对0.20 mg/mL溶菌酶标准溶液进行11次平行测定,RSD为3.82%。结论此法用于人唾液中溶菌酶的含量测定,结果令人满意,方法重复性好,灵敏度高。     

流动注射-抑制化学发光法测定绿茶中的茶多酚含量

茶多酚是茶中的酚类化合物 ,药用价值较高 ,有抗氧化、抗肿瘤、抗动脉粥样硬化、抑菌等药理作用。其测定方法主要有酒石酸亚铁比色法 (标准法 ) [1] 、分光光度法[2 ] 等。流动注射 抑制化学发光法测定茶多酚尚未见报道。本文用茶多酚还原Ｈ2 Ｏ2 ,抑制鲁米诺 Ｈ2 Ｏ2 ＫＩＯ4 体系[3 ] 的化学发光 ,在碱性条件下 ,其抑制程度的大小与茶多酚的含量成线性关系。与其他方法相比 ,本法具有线性范围宽、灵敏度高、简单、快速的优点 ,用于实际样品测定 ,结果令人满意。材料与方法仪器与试剂　ＩＦＦＬ Ｄ型流动注射化学发光仪(西安瑞科电子设…     

流动注射化学发光法测定硫脲的探讨

本文基于 Fe( )氧化硫脲生成 Fe( )的反应和 L uminol- O2 - Fe( )化学发光反应相偶合 ,建立了流动注射化学发光测定硫脲的新方法。方法检出限为 4× 10 - 7mol/ L,RSD=2 % (C=5× 10 - 7mol/ L,n=11) ,方法用于白葡萄酒中硫脲的分析测定 ,结果满意。     

流动注射化学发光法测定醋酸泼尼松

利用醋酸泼尼松对Ｃｅ－Ｎａ２ＳＯ３化学发光体系的增强作用，建立了流动注射化学发光法醋酸泼尼松的新方法。化学发光强度与醋酸泼尼松的浓度在０．２－２０．０ｍｇ／Ｌ范围内呈线性关系，检出限０．０３ｍｇ／Ｌ，对０．２ｍｇ／Ｌ醋酸泼尼松标准溶液的１１次平行测定的相对标准偏差为１．８％。     

鲁米诺—高碘酸钾化学发光法测定盐酸阿朴吗啡

目的:在碱性条件下盐酸阿朴吗啡(Apomorphini Hydrochloridum)对luminol—KIO4化学发光体系具有很强的增敏作用,据此建立了流动注射化学发光法测定盐酸阿朴吗啡新方法。方法:线性范围为5.5×10-3～0.1 mg.L-1,检出限为4.4×10-3mg.L-1,RSD(n=10,c=0.02 mg.L-1)为2.6%,结果:已用于阿朴吗啡在尿样和血样中含量的测定,尿样中的加标回收率为97.32%～104.69%,血样中加标回收率为106.30%～110.57%。结论:由于其易见光分解,需使用合理的前处理手段。     

A novel flow‐injection chemiluminescence method for determination of andrographolide in andrographis tablets

A novel method for determination of andrographolide using flow‐injection chemiluminescence (FI‐CL) analysis is described in this paper. The chemiluminescence intensity of the solution was enhanced proportionally while the concentration of andrographolide increased. Under the selected experimental conditions, the calibration curve of andrographolide was linear within the range of 0.2 to 35.0 µg mL^?1 with a linear equation of ΔI = 23.391x (µg mL^?1) + 34.191, R² = 0.9965. The detection limit (3σ) was 7.42 × 10^?2 µg mL^?1. At the case of continuous determination of andrographolide, the relative standard deviation (RSD, n = 11) was less than 1.82%. The method has been successfully applied to the determination of andrographis tablets with satisfactory results. Copyright © 2012 John Wiley & Sons, Ltd.     

A sensitive flow injection chemiluminescence method for the determination of progesterone

A sensitive flow injection (FI) chemiluminescence (CL) method was developed for the determination of trace amounts of progesterone. This method was based on the luminescent properties of the tris(1,10‐phenanthroline) ruthenium(II) ‐ potassium permanganate (KMnO₄) ‐ progesterone in acidic medium sensitized by Na₂SO₃. With the peak height as a quantitative parameter applying optimum conditions, the relative CL intensity was linear with progesterone concentration in the range of 1.0 × 10^?10 ～ 6.0 × 10^?9 g·ml^?1 and 6.0 × 10^?9 ～ 4.0 × 10^?8 g·ml^?1 with a detection limit of 7.1 × 10^?11 g·ml^?1. The relative standard deviation (RSD) was 2.79% for 1.0 × 10^?8 g·ml^?1 progesterone (n = 11). The proposed method held low detection limit and was successfully applied to determination of progesterone in pharmaceutical preparations. The possible CL reaction mechanism was also discussed. Copyright © 2011 John Wiley & Sons, Ltd.     

高效液相色谱法测定血浆6-巯基嘌呤质量浓度及其药动学

目的：建立血浆中硫唑嘌呤的活性代谢物6-巯基嘌呤质量浓度测定的高效液相色谱分析方法，并研究了6-巯基嘌呤人体药动学。方法：6-巯基嘌呤血浆样品经乙腈沉淀蛋白并行萃取，进一步将有机层吹干富集药品。Hypersil C18柱（4．6mm×150mm，5μm），流动相为乙腈一水（含0．25％醋酸）（3：97），流速1．0mL·min^-1，柱温30℃，检测波长323nm。结果：6-巯基嘌呤在2～200μg·L^-1范围内线性关系良好（r=0．9997），血浆最低检测限度为2μg·L^-1。高、中、低质量浓度（200，50，5μg·L^-1，）的日内及日间RSD均小于8．52％，平均方法回收率分别为98．1％，101．6％和100．8％，平均提取回收率分别为90．2％，94．9％和91）．90％。人体药动学研究表明，口服硫唑嘌呤后6-巯基嘌呤的药一时曲线符合一级吸收的一房室模型。结论：此法灵敏、专一、准确、精密、简便，适用于药动学研究及治疗药物质量浓度监测。     

Coupling reaction and complex formation for the spectrophotometric determination of physiologically active catecholamines in bulk,pharmaceutical preparations and urine samples of schizophrenic patients

A simple and sensitive spectrophotometric method for the determination of three catecholamines namely dopamine hydrochloride (DO.HCl), dobutamine hydrochloride (DOB.HCl) and vanillymandelic acid (VMA), in both pure form or in their commercially available pharmaceutical formulations or urine samples of schizopherinic patients is described. The method is based on the reaction of diazotized 4‐aminoantipyrine (4‐AAP) with catecholamines in a basic medium (pH = 10–11) to yield pink‐coloured products having absorption maxima at 500, 505 and 480 nm for DO.HCl, VMA and DOB.HCl, respectively. Before carrying out Beer's Law, different experimental conditions, such as time, temperature, sequence of addition, and pH are optimized. The coloured species obeyed Beer's Law in the range of 47.4–417.2, 59.45–445.9 and 67.57–405.4 mg/L for DO.HCl, VMA and DOB.HCl, respectively. The molar absorptivity values as obtained from Beer's Law data were found to be 2.979 × 10⁴, 4.39 × 10⁴ and 1.036 × 10⁴ L mol^?1 cm^?1, while Sandell's sensitivity values were observed to be 3 × 10^?3, 4.4 × 10^?3 and 1.3 × 10^?3 µg cm^2? for DO.HCl, VMA and DOB.HCl, respectively. Common excipients did not interfere with the proposed method. The results of the proposed method compare favourably with those of official methods. The proposed method offers simplicity, reliability, rapidity, and accuracy compared to the existing methods. Copyright © 2010 John Wiley & Sons, Ltd.     

An application of Ag(III) complex chemiluminescence system for the determination of enoxacin in capsule and biological fluid

Ag(III) complex chemiluminescence (CL) system was applied for the determination of enoxacin (ENX). The CL conditions of [Ag(HIO(6))(2)](5-)-H(2)SO(4)-ENX systems without any luminescence reagent were investigated and optimized. Under the optimized conditions, the CL intensity was proportional to the concentration of ENX in the range from 6.6 × 10(-5) to 3.3 × 10(-3) g/L. The limit of detection (s/n = 3) was 2.0 × 10(-5) g/L. The recovery of ENX from the spiked pharmaceutical preparations was in the range of 82.9-108% with a relative standard deviation of 1.9-3.0%. For spiked serum and urine samples the recovery of ENX was in the range of 83.7-110% with a relative standard deviation of 1.1-2.8%. The proposed method was applied successfully to the determination of the drug in capsule, serum and urine samples.     

Pharmacokinetics of 6-thiouric acid and 6-mercaptopurine in renal allograft recipients after oral administration of azathioprine

Summary The immunosuppressive activity of azathioprine (AZA) is unpredictable and depends on the formation of intracellular thiopurine ribonucleotides. However, the quantification of these active thiopurines presents difficult analytical problems. It has recently been postulated that plasma concentrations of 6-thiouric acid (6-TU) and 6-mercaptopurine (6-MP), metabolites of AZA, may provide more readily measurable indices of the pharmacologic activity of AZA. In order to evaluate the utility of 6-TU and 6-MP plasma concentrations in monitoring AZA therapy, we studied their pharmacokinetics in 6 renal transplant patients, and their in vitro immunosuppressive potency in a mixed lymphocyte proliferation assay.A peak plasma 6-TU concentration of 710.7 ng/ml was observed at 3.8 h after oral dosing. Good correlation was observed between the elimination t_1/2 of 6-TU and serum creatinine, and between AUC over 24 h and serum creatinine. However, we did not observe a second peak in plasma 6-TU concentration that could be attributed to the degradation of active AZA metabolites. 6-MP plasma concentrations in the patients were low (mean peak concentration 36.0 ng/ml) and rapidly disappeared within 8 h. In vitro immunosuppressive activity could not be demonstrated for 6-TU over a concentration range of 1.25 ng/ml to 0.25 mg/ml.We conclude that 6-TU is pharmacologically inert and is primarily eliminated by the kidneys. Our findings currently do not support the use of plasma concentrations of 6-TU or 6-MP to monitor AZA therapy. In order to optimize AZA therapy, analytical techniques that are technically feasible and that can directly quantify the active intracellular thiopurines are being explored.     

HPLC测定注射用13种维生素中维生素B_6、烟酰胺、D-泛醇的含量

目的:建立同时测定注射用13种维生素中维生素B6、烟酰胺、D-泛醇的HPLC法。方法:采用Diamonsil(TM)C18(250 mm×4.6 mm,5μm)为色谱柱,以20 mmol.L-1磷酸二氢钾(调pH5.0)-甲醇(88∶12)为流动相,流速为1.0 mL.min-1,检测波长为214 nm,柱温为25℃。结果:维生素B6在0.06046~0.2418 mg.mL-1范围内、烟酰胺在0.3999~1.599mg.mL-1范围内,D-泛醇在0.1521~0.6084 mg.mL-1范围内具有良好线性关系;其回收率分别为100.2%,99.8%,100.4%。结论:本方法快速简便,准确可靠,可用于注射用13种维生素中维生素B6、烟酰胺和D-泛醇的质量控制方法。