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脑益嗪的吸附伏安特性及其测定 总被引:1,自引:0,他引:1
在pH2.3的KCl-HCl底液中,脑益嗪在汞电极上有一还原峰。其导数峰电位为-1.47V(SCE);线性范围1.0×10^-7~1.0×10^-6mol/L;最低检测限为1.0×10^-7mol/L。用多种电化学手段证明,脑益嗪的还原属于反应物弱吸附的不同逆过程。该法用于样品中脑益嗪含量的测定,结果令人满意。 相似文献
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A rapid and simple high performance liquid chromatographic method coupled with tandem mass spectrometry (LC–MS–MS) via electrospray
ionization (ESI) has been developed and validated to separate and simultaneously quantify sodium ferulate (SF), salicylic
acid (SA), cinnarizine (CIN) and vitamin B1 (VB1) in human plasma. Gemfibrozil (GEM) was used as the internal standard (IS)
for SF and SA, whereas lomerizine (LOM) was used as the IS for CIN and VB1. The plasma samples were prepared by one-step protein
precipitation followed by an isocratic elution with 10 mM ammonium acetate buffer (pH = 5.0): acetonitrile (35:65, v/v,) on an Agilent Zorbax SB-CN column (150 mm × 2.0 mm ID, 5 μm). The precursor and product ions of these drugs were monitored
on a triple quadrupole mass spectrometer, operating in the selected reaction monitoring mode (SRM) with polarity switch, in
the negative-ion mode for SF, SA and GEM, in the positive-ion mode for CIN, VB1 and LOM. The method was validated over the
concentration range of 1.5–1,000 ng mL−1 for SF, 20–5,000 ng mL−1 for SA, 2–500 ng mL−1 for CIN, 1–30 ng mL−1 for VB1. The intra- and inter-batch precisions were less than 15% of the relative standard deviation. The recoveries for
analytes and IS achieved from spiked plasma samples were consistent and reproducible. The validated LC–MS–MS method has been
successfully applied to the pharmacokinetic study of sodium ferulate and aspirin capsule in healthy volunteers. 相似文献
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Sensitive determination of cinnarizine in human plasma by high performance liquid chromatography and fluorescence detection 总被引:2,自引:0,他引:2
Summary A sensitive high performance liquid chromatographic method has been developed for the determination of cinnarizine in human plasma. Cinnarizine and clocinizine (internal standard) were extracted from acidified plasma (pH 4.7) into carbon tetrachloride and the organic layer was evaporated. The products were separated on a Microspher C18 (3 m) column, using a mixture of 0.04 % triethylamine in 0.01 M ammonium dihydrogen phosphate (NH4H2PO4), pH adjusted to 4.2 with orthophosphoric acid (H3PO4), and acetonitrile (2080, v/v) as mobile phase, at a flow rate of 1 ml/min at 40°C. Fluorescence detection (ex = 245 nm, em = 310 nm) was used; the detection limit was 0.5 ng/ml under the conditions used, and the calibration curve linear in the concentration range evaluated (1–60 ng/ml). The assay has been used to measure cinnarizine concentrations in plasma after oral administration to volunteers. 相似文献
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Manjunatha Hadagali Devagondanahalli Sarfaraj Mohd Takhi Shaikh Seetharamappa Jaldappagari Sudhir Kumar Ramanaboyina Harikrishna Kasalanti 《中国化学会会志》2007,54(1):63-68
Two simple, rapid and sensitive extractive spectrophotometric methods have been developed for the assay of cinnarizine (CNR) in pure and pharmaceutical formulations. The methods are based on the formation of chloroform soluble ion‐association complexes of CNR with thymol blue (TB) and with cresol red (CR) inNaOAc‐AcOH buffer of pH 3.6 for TB and in KCl‐HCl buffer of pH 1.6 for CR with absorption maxima at 405 nm and at 403 nm for TB and CR, respectively. Reaction conditions were optimized to obtain the maximum color intensity. The systems obeyed Beer's law in the range of 0.6–15.8 and 0.8–16.6 μg mL?1 for TB and CR, respectively. Various analytical parameters have been evaluated and the results have been validated by statistical data. 相似文献
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T. Angelov 《Chromatographia》2003,58(7-8):483-485
Summary Cinnarizine is a pharmaceutical drug used in the treatment of cerebral and peripheral vascular diseases. A reversed-phase liquid chromatographic method with fluorescence detection has been developed for determination of the drug in workplace air. Air sampling in the workplace is performed on perchlorovinyl filters (FPP), the filters are extracted with methanol for 40 min, and the extract (50 L) is injected and separated on a 250 mm × 4.6 mm i.d., 5 m particle, C8 reversed-phase column with 1% ammonium acetate (pH 4.5)–acetonitrile, 1:4 (v/v), as mobile phase at a flow rate of 1 mL min–1. 相似文献
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桂利嗪的荷移分光光度法测定 总被引:2,自引:0,他引:2
本研究了桂利嗪与7.7,8,8-四氰基对二次甲苯醌(TCNQ)的荷移(CT)反应,确定了荷移反应的最佳条件。结果表明:在丙酮-甲醇介质中,二于室温条件下10min即可形成1:1的络合物,在其最大吸收波长743nm处表观摩尔吸光系数ε=1.58×10^4L·mol^-1·cm^-1,在0~18μg·mL^-1范围内符合比尔定律。方法的相对标准偏差小于3%(n=10)。对形成CT络合物的机理进行了 相似文献
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A rapid, simple and highly sensitive second derivative synchronous fluorometric method has been developed for the simultaneous
analysis of binary mixture of cinnarizine (CN) and domperidone (DOM). The method is based upon measurement of the native fluorescence
of these drugs at Δλ = 80 nm in aqueous methanol (50% V/V). The different experimental parameters affecting the native fluorescence
of the studied drugs were carefully studied and optimized. The fluorescence-concentration plots were rectilinear over the
range of 0.1 to 1.3 μg mL−1 and 0.1–3.0 μg mL−1 for CN and DOM, respectively with lower detection limits of 0.017 and 5.77 × 10−3 μg mL−1 and quantification limits of 0.058 and 0.02 μg mL−1 for CN and DOM. The proposed method was successfully applied for the determination of the studied compounds in synthetic
mixtures and in commercial tablets. The results obtained were in good agreement with those obtained with reference methods.
The high sensitivity attained by the synchronous fluorometric method allowed the determination of CN in real and spiked human
plasma. The mean % recoveries in case of spiked human plasma (n = 3) were 96.39 ± 1.18 while that in real human plasma (n = 3) was 104.67 ± 4.16. 相似文献
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