氟哌啶醇的吸附伏安法研究

于NH_3-NH_4Cl底液中,氟哌啶醇(Hal)在悬汞电极上有一灵敏的还原蜂。EPC为-1.55V(vs饱和Ag/AgCl电极),其线性扫描吸附伏安法的线性范围为5.0×10~(-9)～9.0×10~(-7)mol/L。最低检测限为2.0×10~(-9)mol/L。测定了用药患者的尿样及针剂,片剂中Hal的含量,结果满意。对Hal在汞电极上的电化学性质,特别是吸附性进行了探讨。     

恶魔背后的天使——杜冷丁的故事

介绍了杜冷丁先生的基本性质及其恶魔面和天使面,以及它在医学各领域中的作用。详细说明了它与其他药物混合使用时的效果,以及当今社会盲目地对杜冷丁等药物过度利用带来的弊端。     

Simple and practicable high-performance liquid chromatographic assay of some tricyclic drugs,haloperidol, diltiazem,verapamil, propafenone and amiodarone

Summary A rapid, practicable and versatile high-performance liquid chromatographic method is described, which applies to different therapeutic drug-monitorings. Using the same extraction procedure with 500μl of serum and 250μl of extracting mixture, the same column and the same mobile phase, the following drugs were separated from endogenous molecules: amitriptyline with nortriptyline, imipramine with desipramine, chlomipramine, haloperidol, diltiazem, verapamil, amiodarone and desethylamiodarone.     

Determination of haloperidol in biological samples with the aid of ultrasound‐assisted emulsification microextraction followed by HPLC‐DAD

A rapid and simple quantitative method for preconcentration and determination of haloperidol in biological samples was developed using ultrasound‐assisted emulsification microextraction, based on the solidification of floating organic droplet combined with HPLC‐DAD. The effects of several factors were investigated. A total of 30 μL of 1‐undecanol as an extraction solvent was injected slowly into a glass‐centrifuge tube containing 4 mL alkaline sample solution that was located inside the ultrasonic water bath. The formed emulsion was centrifuged and the fine droplets of solvent were floated at the top of the test tube, then it was cooled in an ice bath and the solidified solvent was transferred into a conical vial, after melt, the analysis of the extract was carried out by HPLC. Under the optimal conditions, the extraction efficiencies were more than 90% and the preconcentration factors were obtained between 119–122. The LOQs were obtained between 4–8 μg/L and the calibration curves were linear within the range of 4–1000 μg/L. Finally this method was applied to the determination of haloperidol in plasma and urine samples in the range of μg/L and satisfactory results were achieved (RSDs <7%).     

氟哌啶醇的示差脉冲吸附伏安法测定

氟哌啶醇,化学名4-[4-基-4-(4-氯苯)-4-羟基派啶]-4’-氟丁酰苯,是一种重要的抗精神病药。该药物的测定主要采用紫外光度法,其他尚有气相和薄层色谱法,荧光法等。但灵敏度都不够高,难以用于微量和痕量分析,特别是病人体液中含量的监测。 Bishop等发现,氟哌啶醇在金和铂电极上既不还原也不氧化,认为这种药物在上述电极上不具有电活性。本文发现氟哌啶醇能吸附于玻碳电极,并发生氧化反应。据此拟定了吸附伏安法测定该药物的方案,并研究了药物在玻碳表面的吸附行为。     

Microwave-accelerated fluorodenitrations and nitrodehalogenations: expeditious routes to labeled PET ligands and fluoropharmaceuticals

Methods for the expeditious fluorination of arenes have been investigated, using readily available fluoride sources. An optimized procedure for microwave-accelerated fluorodenitration has been developed, giving good to excellent yields in less than 10 min, rendering it practical for use in the preparation of F¹⁸ labeled ligands for PET imaging. Application of the method in the synthesis of CNS agents is demonstrated, and a practical method for the preparation of substrates is also presented.     

Determination of haloperidol and reduced haloperidol in human serum by liquid chromatography after fluorescence labeling based on the Suzuki coupling reaction

A simultaneous method for the determination of haloperidol (HP) and its metabolite, reduced haloperidol (RHP), in human serum was developed by means of high-performance liquid chromatography (HPLC) with fluorescence detection. Suzuki coupling reaction with a fluorescent arylboronic acid, 4-(4,5-diphenyl-1H-imidazol-2-yl)phenylboronic acid (DPA), was employed to convert HP and RHP into highly fluorescent compounds. HP and RHP were extracted from human serum by liquid-liquid extraction with a mixture of n-hexane and isoamyl alcohol (99:1, v/v) and subsequently labeled by reaction with DPA. Separation of DPA derivatives of HP and RHP was performed on a silica column with a mixture of acetonitrile and H(2)O (90:10, v/v) containing triethylamine and acetic acid as a mobile phase. The proposed method allowed sensitive detection of HP and RHP in human serum with a detection limit (at a signal to noise ratio of 3) of 0.22 and 0.20 ng/mL, respectively. The applicability of the method for therapeutic drug monitoring (TDM) was demonstrated by analyzing human serum samples from schizophrenic patients receiving HP.     

Chemical stability of haloperidol injection by high performance thin-layer chromatography

The chemical stability of haloperidol lactate injection was studied under different storage conditions by high performance thin-layer chromatography (HPTLC). The study was performed at 25 +/- 2 degrees C and at refrigeration temperature (8 +/- 1 degrees C) in original glass ampoules over 15 days after being opened. The samples tested at 25 +/- 2 degrees C were stored with exposure to and protection from light. Chromatographic separation was achieved on precoated silica gel F 254 HPTLC plates using a mixture of acetone/chloroform/n-butanol/glacial acetic acid/water (5:10:10:2.5:2.5, v/v/v/v/v) as a mobile phase. Quantitative analyses were carried out at a wavelength of 254 nm. The method exhibited adequate linearity (r = 0.999), selectivity, precision (RSD = 1.92%), and accuracy (recoveries from 98.59 to 101.90%). The concentrations of all samples remained greater than or 90% of the original concentration. Haloperidol lactate injection was chemically stable under all conditions studied over 15 days.     

Changes in proton T1 in dog brains due to the administration of haloperidol

Changes in proton T1 in dog brains due to the administration of haloperidol were determined by the intravenous administration of a single dose of 20 mg of haloperidol to mongrel dogs. The MRI used was the Aberdeen type with the static magnetic field of 0.1 T. A coil made exclusively for these animals (bore diameter 120 mm) was used. There was a significant increase in the T1 value in the striate body 30 minutes and more (within two hours) after the administration of haloperidol. Subtraction images were also obtained by subtracting the image of the pre-treatment (control) T1 values from the image of the post-treatment values (2 hours after the injection). The subtraction images also revealed increases in the T1 values of the striate body.