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Synthesis of magnetic iron oxide nanoparticles and its surface modification with methacrylic acid (MAA) was performed simultaneously by adding Fe(2+)/Fe(3+) to an alkaline MAA solution under nitrogen atmosphere. MAA coated magnetite (Fe3O4@MAA) has abundant reactive double bonds on the surface that can initiate polymerization. Magnetic molecularly imprinted polymers (MMIPs) were synthesized through distillation-precipitation polymerization of MAA as monomer, perphenazine (PPZ) as template, and ethylene glycol di-methacrylate (EGDMA) as cross linker on Fe3O4@MAA, with concise control of experimental conditions in about 90min. The produced super paramagnetic MMIPs can be separated from the solution in the presence of external magnetic field in less than 1min. Characterizations of the synthesized particles were performed by electron microscopes, thermo-gravimetric analysis (TGA), vibrating sample magnetometer (VSM), Fourier transform infrared (FT-IR) spectroscopy, and BET. The data showed that Fe3O4@MAA was well encapsulated in the polymer shell. The MMIPs showed high porosity. Moreover, MMIPs were used for rapid pre-concentration and separation of PPZ in human plasma and urine without any dilution and pretreatments using high performance liquid chromatography equipped with a photo diode array detector (HPLC-PDA). The calibration curve in urine and plasma has shown the same slope as the external calibration curve. Linear range of 20-5000ngmL(-1), and a detection limit of 5.3ngmL(-1) was obtained. The results showed 97.92% recovery along with the relative standard deviation of 6.07% (n=6) for 1μgmL(-1) PPZ. Pre-concentration factor was 13. The MMIPs adsorbed PPZ in 1min and then desorbed it by MeOH:HOAc in 2min., (Copyright © 2016 Elsevier B.V. All rights reserved.)

A luminol-potassium ferricyanide-perphenazine CL reaction with high sensitivity for the determination of perphenazine was found. A perphenazine molecular imprinted polymer (MIP) was synthesized. Using the perphenazine MIP as a recognition material, a novel molecular imprinting-chemiluminescence (MI-CL) sensor for the determination of perphenazine was made based on the luminol-potassium ferricyanide-perphenazine CL reaction. The sensor displayed good selectivity and high sensitivity. The linear-response range of the sensor was 5.0 x 10(-8) - 1.0 x 10(-5) g/ml with a linear correlation coefficient of 0.9961. The detection limit was 2 x 10(-8) g/ml perphenazine and the relative standard deviation for 1.0 x 10(-6) g/ml perphenazine solution was 3.7% (n = 11). The sensor was applied to the determination of perphenazine in urine samples with satisfactory results.

A simple method for determination of perphenazine by capillary zone electrophoresis with amperometric detection is described. The optimum conditions of separation and detection are 1.50 x 10(-3) mol/l Na(2)B(4)O(7)-1.0 x 10(-3) mol/l NaOH (pH 9.9) for the buffer solution, 18 kV for the separation voltage, 5 kV and 5 s for the injection voltage and the injection time, and 0.80 V versus saturated calomel electrode for the detection potential, respectively. The limit of detection is 5.0 x 10(-8) mol/l or 44 amol (S/N=3). The linear range of the calibration curve is 1.00 x 10(-7) to 1.00 x 10(-4) mol/l. The relative standard deviation is 1.5% for the migration time and 2.9% for the electrophoretic current at peak maximum. The method is applied to the determination of perphenazine in human urine.

Perphenazine enanthate has been used in wild animals as a tranquilizer during the period of adaptation to new environments to reduce stress, mortalities and injuries. A gas chromatographic procedure for the quantitative measurement of perphenazine in otter urine has been developed and validated. The method involved an enzymatic hydrolysis with beta-glucuronidase-arylsulfatase from Helix pomatia, followed by a solid-phase extraction with Bond Elut Certify cartridges. The resulting organic phase was evaporated, and the dry extract was derivatised with MSTFA to form the O-TMS derivative. The derivatised extracts were analysed by gas chromatography-mass spectrometry using SIM acquisition mode, measuring three diagnostic ions (m/z 246, 372 and 475). Another phenothiazine derivative, fluphenazine, was used as the internal standard (I.S.). Extraction recoveries for perphenazine and I.S. were 87.6 +/- 8.2% (n=4) and 106.7 +/- 13.4% (n=4), respectively. The calibration curves were linear in the range from 4 to 100 ng/ml (r2=0.99). The limits of detection and quantification were estimated as 1.2 and 3.5 ng/ml, respectively. Precision and accuracy obtained in intra-assay studies were in the ranges of 1.3-8.7 and 1.7-19.5%, respectively, using control samples containing 6, 16 and 60 ng/ml of perphenazine. In inter-assay experiments, precision ranged from 4.3 to 14.9% and accuracy from 3.1 to 11.8%. Examples of the application of the perphenazine quantification method in otter urines after administration of perphenazine enanthate are presented.