CdTe量子点荧光猝灭法测定尼群地平的研究

以L-半胱氨酸为稳定剂,在水溶液中合成了CdTe量子点.以该量子点为荧光探针,基于荧光猝灭法对尼群地平进行了定量检测.考察了缓冲体系、缓冲液浓度、缓冲液pH值、反应时间、量子点浓度等多种因素的影响,并对反应机理进行了初步的探讨.在0.03 mol/L、pH值为5.78的Tris-HCl缓冲液中,当量子点浓度为5.72×10-4mol/L、反应时间为10 min时,该方法的线性范围为0.38~77μg/mL,检出限为0.28μg/mL.该方法已成功用于药片中尼群地平的测定,与中国药典中的标准方法比较,结果满意.     

Validated LC–MS/MS method for the simultaneous determination of enalapril maleate,nitrendipine, hydrochlorothiazide,and their major metabolites in human plasma

Hypertension is a major risk factor for atherosclerosis and ischemic heart disease. Most hypertensive patients need a combination of antihypertensive agents to achieve therapeutic goals. A rapid, sensitive, and selective liquid chromatography-tandem mass spectrometric method was developed and validated for simultaneous determination of enalapril maleate (ENA) and its major metabolite enalaprilat (ENAT), nitrendipine (NIT) and its major metabolite dehydronitrendipine (DNIT), and hydrochlorothiazide (HCT) in human plasma using felodipine as an internal standard (IS). The drugs were extracted from plasma using one-step protein precipitation. Chromatographic separation was performed on a Symmetry C₁₈ column, with water and acetonitrile (10:90, v/v) as mobile phase. The detection was carried out using multiple reaction monitoring mode and coupled with electrospray ionization source. Multiple reaction monitoring transitions were m/z 377.1 → 234.1 for ENA, m/z 349.2 → 206.1 for ENAT, m/z 361.2 → 315.1 for NIT, m/z 359 → 331 for DNIT, m/z 295.9 → 205.1 for HCT, and m/z 384.1 → 338 for felodipine (IS). The method was linear over concentration ranges of 1–200, 20–500, 5–200, 2–100, and 5–200 ng/mL for ENA, ENAT, NIT, DNIT, and HCT, respectively, with r² ≥ 0.99. Method validation was performed according to U.S. Food and Drug Administration guidelines. The validated method showed good sensitivity and selectivity and could be applied for therapeutic drug monitoring and bioequivalence studies.     

差分脉冲伏安法同时检测硝苯地平和尼群地平

采用绿色环保的还原剂聚二烯丙基二甲基氯化铵,制备石墨烯(GR)/聚二烯丙基二甲基氯化铵(PD-DA)/铂纳米粒子(PtNPs)复合材料,在此基础上制备了GR/PDDA/PtNPs复合修饰电极,并采用透射电镜、电化学等方法对GR/PDDA/PtNPs进行表征.以pH=8.5的B.R缓冲溶液为支持电解质,采用循环伏安法研究...     

水溶性CdTe量子点荧光猝灭法测定尼群地平的研究

以巯基乙酸为稳定剂,直接合成了水溶性CdTe量子点。基于尼群地平对合成量子点的荧光猝灭效应,建立了一种简便、快速和灵敏地测定尼群地平的分析方法。考察了缓冲体系、缓冲液浓度、缓冲液pH值、反应时间、量子点浓度对尼群地平测定的影响,在0.03 mol/L、pH值为8.3的Tris-HCl缓冲液中,当量子点的浓度为6.0×10-4mol/L、反应时间为5 min,体系的相对荧光强度与尼群地平的质量浓度呈良好线性关系,其线性范围为1.09~65.4 mg/L,线性系数为0.998 6,检出限(S/N=3)为0.11 mg/L。该方法已成功用于药片中尼群地平的测定,与中国药典中的标准方法比较,结果满意。同时该文对尼群地平与CdTe量子点的反应机理进行了初步探讨。     

尼群地平晶型转变条件及其影响因素的确定

根据熔化数据推算相变稳定性理论计算了尼群地平不同晶型之间的相变温度, 并分别考察了高温、高温和高湿及高压条件下的晶型转变. 理论推导尼群地平I与II, 尼群地平I与III, 尼群地平II与III的转化温度分别为158.88, 160.50和158.65 ℃, 三者均为单变关系, 且在高温条件下尼群地平II, III都转变为尼群地平I, 在高压条件下, II易转变为I. 试验结果表明室温下尼群地平I为稳定型, II和III为亚稳定型, 3种晶型稳定性顺序为尼群地平I＞II＞III.