共振瑞利散射光谱法测定血浆和尿样中的帕珠沙星

目的建立了共振瑞利散射光谱法测定血浆、尿样中帕珠沙星含量的新方法。方法于pH4.8～5.9的Britton-Robinson缓冲溶液中,帕珠沙星与钴(Ⅱ)形成阳离子配合物,其共振瑞利散射(resonance rayleigh scattering,RRS)十分微弱,但当其进一步通过静电引力和疏水作用与刚果红(congo red,CR)阴离子反应形成三元离子缔合物时,RRS出现新的共振瑞利散射光谱,其2个散射峰分别位于380和562nm处。结果在380nm处,帕珠沙星的质量浓度在0.031～3.18μg.mL-1范围内,与RRS强度有良好的线性关系,其检出限(3σ)为24.6ng.mL-1。结论该方法简单、快速,具有良好的选择性和重复性,可用于不同体液中帕珠沙星的测定。     

透明质酸钠-溴化十六烷基吡啶缔合物体系的共振瑞利散射光谱及其应用

在pH 4.3的Britton-Robinson缓冲溶液中,透明质酸钠和溴化十六烷基吡啶各自单独存在时,共振瑞利散射(RRS)强度非常弱,但当两者反应形成离子缔合物时,RRS大大增强并产生新的RRS光谱,最大RRS峰位于335 nm处.透明质酸钠在0.1～3.0 μg/ml浓度范围内与RRS强度成正比.据此,建立了共振瑞利散射光谱法测定透明质酸钠,检测限为29ng/ml.     

共振瑞利散射光谱法测定片剂、人体尿液和血浆中培氟沙星的含量

目的 建立测定片剂、人体尿液和血浆中的培氟沙星含量的共振瑞利散射光谱方法.方法 在pH4.8～5.9 Britton-Robinson缓冲溶液中,培氟沙星(PEFX)可与钴(Ⅱ)反应形成配阳离子,其共振瑞利散射(RRS)十分微弱,但当该配阳离子进一步与酸性染料刚果红(CR)阴离子反应形成三元离子缔合物时,RRS显著增强,3个散射峰别位于278、380和560nm,以380nm为测定波长.结果 线性范围为0.133～3.33μg/mL(r=0.9993),检出限(3σ)为26.4ng/mL.结论 方法简单、快速、并有良好的选择性,可用于片剂、人体尿液和血清中培氟沙星的测定.     

共振瑞利散射法测定多柔比星脂质体中游离多柔比星的含量

目的:建立共振瑞利散射法(RRS)测定多柔比星(DOX)脂质体中游离 DOX 含量。方法:在 pH 2.6的 Britton-Robinson(BR)缓冲液中,刚果红(CR)与 DOX 通过分子间作用力形成离子缔合物,在λ_(ex)=λ_(em)=380 nm 波长时能使 RRS 信号显著增强。结果:RRS 法在1～12 μg·mL~(-1)范围内呈线性关系,检出限为0.05~(-1)g·mL~(-1)。对6个不同批号的 DOX 脂质体混悬液中游离 DOX 的含量测定,结果与紫外可见分光光度法相符,RSD(n=6)为1.9%～3.2%,平均回收率为94.3%。结论:此方法灵敏度较高,可以用于测定 DOX 脂质体中游离 DOX 的含量。     

藻红可见吸收光谱法测定药片中的盐酸美西律

目的 建立快速测定药物中盐酸美西律的高灵敏可见吸收光谱法。方法 在酸性Tris-HCl 介质中,利用藻红与盐酸美西律的显色反应生成具有2 个较强正吸收峰的离子缔合物,采用单波长（SWO）和双波长(DWO) 可见吸收光谱法研究药物中盐酸美西律的定量检测方法,测定波长为477 nm 和548 nm。结果 在pH 4.69 的酸性溶液中,藻红与盐酸美西律通过静电引力相互作用生成二元离子缔合物,使吸收曲线出现2 个较强的正吸收峰,分别位于477 nm 和548 nm,盐酸美西律在0.03～4.3 mg/L 范围内的质量浓度与吸光度（A477 和A548）呈好的线性关系,服从朗伯-比尔定律,单波长法的表观摩尔吸光系数(κ)为5.56×104 L/(mol?cm)（477 nm） 和5.04×104 L/(mol?cm)（548 nm）,检出限分别为0.024 mg/L（477 nm）和0.020 mg/L（548 nm）。双波长法的表观摩尔吸光系数(κ) 达1.05×105 L/(mol?cm),检出限为0.011 mg/L,回收率为98.4%～102%,相对标准偏差为2.2%～2.6%。结论 单波长或双波长可见吸收光谱法均可用于药物中盐酸美西律的定量测定,且简便、快速、灵敏。     

维多利亚蓝B共振光散射光谱法测定利福平

目的 建立测定痕量利福平的高灵敏共振瑞利散射法.方法 在弱碱性Tris-盐酸缓冲介质中,维多利亚蓝B与利福平反应后生成的络合物能使共振瑞利散射显著增强,在345nm处,增强的共振光散射强度△IRRS与一定浓度范围的利福平线性相关.结果 在345nm处,利福平的质量浓度在0.016～0.83mg/L范围内与△IRRS成正比,方法的检出限(3Sb/S)为0.0029mg/L.结论 本方法用于尿样及市售利福平药物中利福平含量的测定,RSD小于1.2％,样品加标回收率为98.5％100.6％,结果满意.     

茜素共振瑞利散射法测氯霉素的含量

目的建立测定痕量氯霉素的共振瑞利散射法。方法以茜素作探针的共振瑞利散射法测定氯霉素。结果在pH 7.12的Tris-HCl缓冲溶液中,氯霉素和茜素相互作用后,共振瑞利散射显著增强,在373nm处的△IRRS最强。氯霉素的质量浓度在0.097~0.32mg/L范围内与△IRRS成正比,检出限(3Sb/S)为0.080mg/L。结论该法用于氯霉素注射液、滴眼液中氯霉素的测定,结果满意。实现了以廉价试剂、简便方法快速测定痕量药品的目的 。     

共振瑞利散射法测定透明质酸

目的 建立透明质酸钠的共振瑞利散射（RRS）测定方法。方法于10ml比色管中依次准确加入一定量的钠盐（SH）标准溶液、1．0mlpH5．0的HAc-NaAc缓冲溶液和2ml0．01％的CV溶液,以二次蒸馏水定容,摇匀。将溶液于荧光光度计上以入em=入ex（即△入=0）方式进行同步扫描得RRS光谱,于入em=入ec处测定产物溶液的散射光强度Ⅰ和试剂空白的散射强度Ⅰ0,以△Ⅰ=Ⅰ—Ⅰ0计量记录。结果透明质酸钠与结晶紫在pH3．6～5．6的HAc—Ac^-酸性介质中作用,将导致其溶液的共振瑞利散射（RRS）增强,并产生新的RRS光谱,其最大散射峰位于341nm处。在0—2．0mg／L范围内透明质酸钠浓度与RRS强度成正比。透明质酸钠的检出限（3σ）为17．1ng／ml,RSD为2．1％。结论 该法灵敏度高,选择性也较好。用于测定从动物组织鸡冠中提取自制的透明质酸粗品,结果满意。     

共振瑞利散射法测定微量唑来膦酸

建立了共振瑞利散射法测定微量唑来膦酸。在酸性条件下,唑来膦酸被破坏后产生的无机磷进一步与钼酸铵结合形成磷钼杂多酸,再与罗丹明B形成磷钼杂多酸-罗丹明B三元离子缔合物后共振瑞利散射急剧增加,并于370nm处有最大散射峰,唑来膦酸在6.25～100ng/ml浓度范围内线性关系良好,检测限为1.55ng/ml。     

小檗碱-四苯硼钠缔合纳米微粒体系的共振Rayleigh散射光谱及其分析应用小檗碱-四苯硼钠缔合纳米微粒体系的共振Rayleigh散射光谱及其分析应用

目的研究(小檗碱-四苯硼钠)_n缔合纳米微粒的形成与共振Rayleigh散射之间的关系，建立测定小檗碱的共振Rayleigh散射光谱分析新方法。方法采用共振Rayleigh散射光谱法、吸收光谱和透射电镜研究四苯硼钠(TPB)与盐酸小檗碱(BB)的缔合反应。结果在pH 5.0 NaAc-HAc缓冲溶液中，TPB与BB结合形成的(BB-TPB)_n缔合纳米微粒在470 nm处产生一个共振Rayleigh散射（RRS）峰。建立了测定0.06～5.28 mg·L^-1盐酸小檗碱的RRS新方法，检出限为26 μg·L^-1。 结论通过TPB－与BB⁺和Ag⁺反应形成可用透射电镜观测的(BB_jAg_p-TPBj+p)h复合缔合纳米微粒，证实了固液界面的形成是导致其共振Rayleigh散射光增强的充分必要条件。建立的RRS新方法可用于中成药中微量小檗碱的测定，具有灵敏度高，试样用量少等特点。     

A sensitive and simple method for the determination of chondroitin sulfate a with crystal violet by resonance rayleigh scattering technique

Resonance Rayleigh scattering (RRS) spectra resulting from interaction between chondroitin sulfate A (CSA) and crystal violet (CV) have been investigated and applied to the determination of CSA. Though the intensity of RRS has proved very weak for CSA and CV, respectively, it can be greatly enhanced when both interact and form a supramolecular complex. A new RRS spectrum appears with a maximum scattering peak at 328 nm. In this paper, the optimum conditions of the interaction, influencing factors, and the relationship between the relative intensity of RRS (DeltaI) and the concentration of CSA have been thoroughly investigated. A new method of determination for the trace amount of CSA has been developed, which combines a simple procedure, high sensitivity, and a low detection limit of 4.8 ng/mL. It has been applied with satisfactory results to the determination of CSA in CSA injection samples and synthetic samples.     

阿莫西林与甲基紫的共振瑞利散射及应用

目的建立测定痕量阿莫西林的共振瑞利散射法。方法以甲基紫作探针的共振瑞利散射法测定阿莫西林。结果在pH 9.90的Tris-HCl溶液中,阿莫西林和甲基紫相互作用后,共振瑞利散射显著增强,在376 nm处的△IRRS最强。阿莫西林的浓度在2.0×10-8~1.5×10-6 mol.L-1内与△IRRS成正比,检出限（3Sb/S）为0.042μg.mL-1。结论该法简便、快速、灵敏,可用于痕量阿莫西林的测定。     

A highly sensitive resonance Rayleigh scattering method for the determination of bleomycinA5 and bleomycinA2 with some halofluorescein dyes

In a weak acidic medium, bleomycinA(5) (BLMA(5)) and bleomycinA(2) (BLMA(2)) can react with halofluorescein dyes such as erythrosine (Ery), eosin Y (EY), eosin B (EB) and Rose Bengal (RB) by virtue of electrostatic attraction and hydrophobic force to form ion-association complexes, which can result in the large-scale enhancement of resonance Rayleigh scattering (RRS) and the appearance of new RRS spectra. The increments of scattering intensity (Delta I) were directly proportional to the concentrations of bleomycin (BLM) in certain ranges. The detection limits for BLMA(5) and BLMA(2) ranged from 0.017 to 0.062 microg ml(-1). The Ery system had the highest sensitivity and its detection limit (3sigma) was 0.017 microg ml(-1) for BLMA(5) and 0.018 microg ml(-1) for BLMA(2), respectively. Using Ery as a RRS probe, a new highly sensitive method for the determination of BLM anticancer drugs has been developed. It was applied in the determination of BLMA(5) and BLMA(2) in serum and urine samples. The recovery was from 99.0% to 103.0%. In this work, the RRS spectral characteristics of the binding products and the optimum conditions of the reaction were investigated. The mechanism of ion-association reaction and the reasons of enhancement of resonance light scattering were discussed.     

Determination of the particle size of realgar nano-particles by scanning 

目的：建立纳米雄黄的粒度分析研究方法。方法：利用扫描电镜对纳米雄黄表观形态进行直接观察测定,用激光光散射法对纳米雄黄的粒度分布范围进行分析测定。结果：经扫描电镜和激光光散射颗粒度测定仪的测量,粒径在100 nm以下的纳米雄黄约达90%,其中较大颗粒又是由粒径在5~30 nm左右的细小晶粒和其周围的非晶体聚集而成。结论：扫描电镜法和激光光散射法快速、简便、准确,可用于纳米雄黄的粒度检测。     

当归和欧当归中藁本内酯的薄层扫描测定法

藁本内酯(Ligustilide)是当归(Angelica sinensis Diels)和欧当归(Livisticum officinale koch)根挥发油中的主要成分。已报道当归和欧当归挥发油中含藁本内酯分别约为60％和35％。三桥博等人报道藁本内酯是一种新的活性物质。两种挥发油有相似的药理活性,对大鼠离体子宫有抑制其节律性收缩的作用。     

Voltammetric behaviour of rabeprazole at a glassy carbon electrode and its determination in tablet dosage form

The oxidative behaviour of rabeprazole was studied at a glassy carbon electrode in Britton-Robinson (BR) buffer solutions using cyclic, linear sweep and differential-pulse voltammetry. The oxidation process was shown to be irreversible over the pH range (6.0-11.0) and was diffusion-adsorption controlled. An analytical method was developed for the determination of rabeprazole in BR buffer solution at pH 8.0 as supporting electrolyte. The anodic peak current varied linearly with rabeprazole concentration in the range 1.0 x 10(-6) to 2.0 x 10(-5) M of rabeprazole with a limit of detection of 4.0 x 10(-7) M. Validation parameters, such as sensitivity, accuracy, precision and recovery, were evaluated. The proposed method was applied to the determination of rabeprazole in the tablet dosage form. The results were compared with those obtained by a published high-performance liquid chromatographic method. No difference was found statistically.