脑益嗪的吸附伏安特性及其测定

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。     

Simultaneous Quantification of Sodium Ferulate, Salicylic Acid, Cinnarizine and Vitamin B1 in Human Plasma by LC Tandem MS Detection

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.     

Sensitive determination of cinnarizine in human plasma by high performance liquid chromatography and fluorescence detection

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.     

少量水存在下桂利嗪和茜素在甲醇中的荷移反应

研究了在少量水存在下桂利嗪和茜素在甲醇介质中的电荷转移反应,确定了最佳反应条件。研究表明,反应生成1∶1型荷移络合物,该络合物的λmax=527nm,表观摩尔吸光系数ε=2.94×103L·mol-1·cm-1,桂利嗪浓度在25～200mg/L范围内符合比尔定律,相对标准偏差为1.55%(n=6),平均回收率在98%以上。     

Determination of Cinnarizine in Pure and Pharmaceutical Formulations

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.     

High-Performance Liquid Chromatographic Determination of Cinnarizine in Workplace Air

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.     

桂利嗪的荷移分光光度法测定

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     

Second-derivative Synchronous Fluorometric Method for the Simultaneous Determination of Cinnarizine and Domperidone in Pharmaceutical Preparations. Application to Biological Fluids

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.