双嘧达莫的荧光光谱分析法

以荧光光谱法研究了双嘧达莫在溴化十六烷基三甲基铵(CTMAB)、β_环糊精 (β_CD)、十二烷基硫酸钠 (SDS)等介质体系中的荧光性质 ,发现CTMAB、SDS和 β_CD对双嘧达莫均有不同程度的荧光增敏作用 ,提出了在CTMAB、SDS和 β_CD水溶液中测定双嘧达莫的荧光光谱分析法 ;该法灵敏度高 ,检出限低(3.20×10 -9mol/L) ,在6.40×10 -8～3.20×10 -6mol/L范围内荧光强度与双嘧达莫的浓度呈良好线性关系     

Development and validation of a stability-indicating HPLC method for the determination of degradation products in dipyridamole injection

Summary The development and subsequent validation of an isocratic high-performance liquid chromatographic (HPLC) procedure employing ultraviolet (UV) detection for the determination of degradation products in Dipyridamole Injection is reported. The development of this assay involved the evaluation of several factors including buffer type, ionic strength, pH, organic composition, and column type. The described method is simple, reproducible, accurate, and selective. The precision, relative standard deviation (RSD), amongst five sample preparations for total degradation products was not more than (NMT) 10.2 %, while the individual degradation products were NMT 12.1%. Intermediate precision, as determined from fifteen sample preparations, generated by two Analysts on different HPLC systems over three days, exhibited an RSD for total and individual degradation products of 8.2 % and NMT 27.5 %, respectively. The mean absolute recovery of dipyridamole using the described method is 102.1±1. 9%, (mean±SD, n=12) over the concentration range of 0.03 % to 5.0 % of its label claim of 5 mg mL⁻¹. The limit of detection and limit of quantitation were 0.1 and 0.3 μg mL⁻¹, respectively. The linearity of the peak response was verified with respect to dipyridamole concentration over a range of 0.3 and 50 μg mL⁻¹ (0.03 % to 5.0 % label claim). The Standard and Assay Preparations are stable for up to 48 hours at room temperature. The selectivity was evaluated by subjecting the finished product (Dipyridamole Injection) to thermal, acidic, basic, oxidative and fluorescent radiation stress conditions. No interference in the analysis of degradation products was observed, showing the method is stability-indicating.     

铁氰化钾-鲁米诺体系后化学发光反应及其分析应用研究-分子印迹-后化学发光法测定双嘧达莫

研究了双嘧达莫在铁氰化钾-鲁米诺化学发光反应体系中的后化学发光反应, 并在研究其反应的动力学性质、化学发光光谱、荧光光谱以及一些相关问题的基础上, 探讨了反应机理; 合成了双嘧达莫的分子印迹聚合物, 以此聚合物为分子识别物质, 利用铁氰化钾-鲁米诺-双嘧达莫后化学发光体系, 建立了测定双嘧达莫的高选择性分子印迹-后化学发光分析方法. 所建方法的线性范围为1.0×10-8-1.0×10-6 g/mL(r=0.999 2), 检出限为3×10-9 g/mL, 相对标准偏差为2.7%(1.0×10-7 g/mL双嘧达莫, n=11).     

荧光光度法测定胰腺肿瘤细胞膜上的潘生丁

测定了胰腺肿瘤细胞膜上的潘生丁在乙腈 -水溶液中的荧光光谱和强度 ,并推算出胰腺肿瘤细胞膜上核苷载体的数量。潘生丁的浓度与其荧光强度在 1.0× 10 -12 — 5 .0× 10 -5mol/ L范围内呈线性关系 ,检出限为 2 .8× 10 -13 mol/ L(1.4× 10 -4ng/ m L) ,相对标准偏差为 2 .7%。     

Spectrophotometric Determination of Ternary Mixtures by the Derivative Ratio Spectrum-Zero Crossing Method

Abstract

A new spectrophotometric method is introduced for the assay of ternary mixtures with overlapping spectra. The method is based on the use of the first derivative of the ratio spectra and measurements of zero-crossing wavelengths. The ratio spectra were obtained by dividing the absorption spectrum of the mixture by that of one of the components. The concentration of the other components are then determined from their respective calibration graphs treated similarly. The method has been applied for the resolution of two ternary mixtures, namely, dipyridamole, aspirin and salicylic acid (I) and dipyridamole, oxazepam and 2-amino-5-chlorobenzophenone (II). Salicylic acid and benzo-phenone derivative are the degradation products of aspirin and oxazepam, respectively. The proposed method was applied for the assay of these combinations in synthetic mixtures and in commercial dosage forms. The results obtained were precise and accurate.     

鲁米诺-铁氰化钾化学发光体系测定双嘧达莫

在碱性条件下,铁氰化钾氧化鲁米诺产生化学发光,双嘧达莫对该体系的化学发光有显著的增强作用。基于此并结合流动注射技术建立了测定双嘧达莫的新方法。该方法检出限为5.7×10-11g mL(IUPAC),线性范围为1.0×10-10～5.0×10-8g mL,对5.0×10-9g mL双嘧达莫平行测定11次,其相对标准偏差为1.9%。     

新型涂碳式双嘧达莫选择电极的研制与应用

报道了一种以双嘧达莫与碘化铋形成的缔合物为电活性物的新型涂碳式PVC膜双嘧达莫选择电极,测定了双嘧达莫片的含量。电极线性响应范围为1.0×10-2~2.2×10-5mol/L,级差电位为48 mV/pc,检出限为1.8×10-5mol/L。该电极响应迅速,重现性好,分析结果与药典法相符。     

流动注射化学发光法测定双嘧达莫

采用流动注射技术研究了酸性条件下,双嘧达莫与高锰酸钾和过氧化氢的化学发光行为,对影响化学发光强度的诸因素进行了实验和探讨,建立了流动注射化学发光法测定双嘧达莫的新方法。方法的检出限为5．8×10-8g／mL,线性范围为2×10-7～8×10-5g／mL,对4×10-6g/mL双嘧达莫进行了11次平行测定,相对标准偏差为1．4％。方法用于药剂中双嘧达莫含量的测定,结果与药典标准法测得值一致。     

基于分子印迹识别的化学发光微流控传感器芯片测定双嘧达莫

试验中,以双嘧达莫为模板分子,α-甲基丙烯酸为功能单体,乙二醇二甲基丙烯酸酯为交联剂,氯仿为溶剂,合成了双嘧达莫分子印迹聚合物。将此聚合物填充在长8 mm,宽1 mm,深0.5 mm的微流控芯片检测池中作为分子识别物质,设计了一种新型的化学发光微流控传感器芯片测定双嘧达莫。双嘧达莫被此聚合物在线吸附并识别,被吸附的双嘧达莫与鲁米诺和铁氰化钾混合溶液反应并导致其化学发光强度增大。该传感器对双嘧达莫响应范围为1.0～20μg·L~(-1),检出限(3σ)为0.5μg·L~(-1),对10μg·L~(-1)双嘧达莫连续平行测定7次,其相对标准偏差为4.6%。     

Potentiometric Dipyridamole Sensors Based on Lipophilic Ion Pair Complexes and Native Ionic Polymer Membranes

Abstract

A new spectrofluorimetric method was developed for the determination of trace amounts of lecithin. Using enoxacine (ENX)‐terbium ion (Tb³⁺) as a fluorescent probe, in a buffer solution at pH=5.80, lecithin can remarkably reduce the fluorescence intensity of the ENX‐Tb³⁺ complex at λ=545 nm; the reduced fluorescence intensity of the Tb³⁺ ion is proportional to the concentration of lecithin. Optimum conditions for the determination of lecithin were also investigated. The linear range and detection limit for the determination of lecithin were 1.96×10^?7–9.8×10^?6 mol l^?1 and 9.74×10^?8 mol l^?1. This method is simple, practical and relatively free of interference from coexisting substances, and can be successfully applied to assess lecithin in serum samples.