scholarly journals Determination of Chlorpromazine in Serum by Radioreceptor Assay and HPLC

1986 ◽  
Vol 23 (3) ◽  
pp. 340-345 ◽  
Author(s):  
J Krska ◽  
G M Addison ◽  
S D Soni
Keyword(s):  
Parent Drug ◽  
Hplc Method ◽  
Radioreceptor Assay ◽  
Serum Prolactin ◽  
Active Metabolites ◽  
Serum Prolactin Level ◽  
Serum Samples ◽  
Blocking Activity ◽  
Schizophrenic Patients

A radioreceptor assay for chlorpromazine in serum, which is based on binding to dopamine receptors, is described. This method has been postulated to measure all active metabolites as well as the parent drug. We have compared this method with an HPLC method for chlorpromazine. Dopamine-blocking activity, measured in serum samples from schizophrenic patients receiving chlorpromazine, was 1·85–9·1 times higher than serum chlorpromazine level measured by HPLC. The correlation between the two methods was 0·75. Dopamine-blocking activity was related more closely to dose of drug and to serum prolactin level than was serum chlorpromazine level measured by HPLC.

Simultaneous Determination of Chloroquine and Pyrimethamine with Cetirizine in an Active Form and Human Serum by RP-HPLC

2021 ◽  
Author(s):  
Hina Shamshad ◽  
Ali Sayqal ◽  
Jahan Zeb ◽  
Agha Zeeshan Mirza
Keyword(s):  
Human Serum ◽  
Simultaneous Determination ◽  
Active Form ◽  
Internal Standard ◽  
Hplc Method ◽  
Serum Samples ◽  
Rp Hplc ◽  
Cetirizine Hydrochloride ◽  
Bulk Drug

Abstract A simple, accurate and precise RP-HPLC method was developed for the simultaneous determination of chloroquine, pyrimethamine and cetirizine hydrochloride concentrations in bulk drug and human serum. The assay was performed using a mobile phase of methanol: water (70:30) at pH of 2.8 ± 0.05 on the Purospher C-18 column with UV detection at 230 nm and rosuvastatin used as an internal standard. The retention times observed for chloroquine, pyrimethamine and cetirizine hydrochloride were 3.5, 2.5 and 5.5 minutes, respectively. The method was found to be specific for the assayed drugs showing a linear response in the concentration range of 1–100 μg mL−1 with coefficients of determination values of (r = 0.999). The method was developed and validated according to ICH guidelines. The method was used to monitor the serum samples and was found to be sensitive for therapeutic purposes, showing the potential to be a useful tool for routine analysis in laboratories.

scholarly journals Direct Injection Liquid Chromatographic Technique for Simultaneous Determination of Two Antihistaminic Drugs and Their Main Metabolites in Serum

2007 ◽  
Vol 90 (2) ◽  
pp. 384-390 ◽  
Author(s):  
Samy Emara ◽  
Alaa El-Gindy ◽  
Mostafa K Mesbah ◽  
Ghada M Hadad
Keyword(s):  
Human Serum ◽  
Simultaneous Determination ◽  
Chromatographic Technique ◽  
Simple Liquid ◽  
Good Precision ◽  
Active Metabolites ◽  
Serum Samples ◽  
Antihistaminic Drugs ◽  
Liquid Chromatographic

Abstract A very simple liquid chromatographic technique was developed and validated for the simultaneous determination of 2 antihistaminic drugs, loratadine (LT) and terfenadine (TR), and their major active metabolites, desloratadine (DL) and fexofenadine (FX), respectively, in human serum. LT, DL, TR, and FX from directly injected serum samples were enriched on a protein-coated RP8 silica precolumn (10 4.6 mm id) while serum constituents, such as proteins and salts, were eluted to waste. Using an online column-switching system, the drugs and their metabolites were quantitatively transferred and separated on a second analytical column (Shim-pack 5 μm particle size cyanopropyl, 250 × 4.6 mm id) followed by ultraviolet detection at 243 nm for LT and DL and 220 nm for TR and FX. Very good precision, accuracy, and linearity were obtained over the range of 101000 ng/mL for LT and DL, 10500 ng/mL for TR, and 103000 ng/mL for FX in human serum. High extraction recoveries from serum ranging from 96.03 to 98.19, 95.44 to 97.26, 95.61 to 98.17, and 95.60 to 97.89 for LT, DL, TR, and FX, respectively, were obtained.

Development and validation of a radioreceptor assay for the determination of morphine and its active metabolites in serum

2005 ◽  
Vol 39 (5) ◽  
pp. 964-971 ◽  
Author(s):  
Lutea A.A. de Jong ◽  
Katharina Krämer ◽  
Marieke P.H. Kroeze ◽  
Rainer Bischoff ◽  
Donald R.A. Uges ◽  
...  
Keyword(s):  
Radioreceptor Assay ◽  
Active Metabolites ◽  
Development And Validation

scholarly journals Determination of diazepam and its metabolites in serum by the use of liquid chromatography: Mass spectrometry method

2007 ◽  
Vol 64 (10) ◽  
pp. 659-662 ◽  
Author(s):  
Snezana Djordjevic ◽  
Vesna Kilibarda
Keyword(s):  
Biological Fluids ◽  
Accurate Method ◽  
Reversed Phase ◽  
Active Metabolites ◽  
Serum Samples ◽  
Standard Curve ◽  
Routine Identification ◽  
Selective Ion Monitoring ◽  
Pharmacologically Active

Background/Aim. Diazepam is a benzodiazepine anxyolitic. Metabolism of diazepam takes place in liver which generates pharmacologically active metabolites N-desmethyldiazepam, temazepam and oxazepam. The aim of this study was to develop and validate the method of liquid chromatographymass spectrometry (LC-MS) for separation and determination of diazepam and its active metabolites in the serum of rats samples after i.p. application of diazepam in a dose of 10 mg/kg. Methods. The serum samples taken from Wistar rats, were used in LC-MS analysis after the application of 10 mg/kg of diazepam i.p. Results. After alkaline extraction from the serum samples with diethylether and separation on a C18 reversed-phase column by using mobile phase methanolglacial acetic acid-water (50:1:49 v/v), diazepam and its metabolites were quantified. Determination was performed in a selective ion monitoring (SIM) mode, thereby the other exogenous and endogenous compounds did not interfere with this assay. Diazepam, N-desmethyldiazepam, oxazepam and temazepam were eluted in 14 minutes. The standard curve was linear in the range from 10-2 000 ng/ml. The limits of detection for diazepam, N-desmethyldiazepam, oxazepam and temazepam were 4.37, 3.13, 4.38 and 7.31 ng/ml, respectively. The limits of quantitation for diazepam, Ndesmethyldiazepam, oxazepam and temazepam were 14.58, 10.41, 14.59 and 24.36 ng/ml, respectively. Conclusion. The described LC-MS is a simple, sensitive, specific and accurate method and could be used for routine identification and quantification of small concentrations of diazepam and its metabolites in biological fluids.

Development and Validation of an RP-HPLC Method for Determination of Atorvastatin and its Hydroxyl Metabolites in Human Plasma

2020 ◽  
Vol 16 (3) ◽  
pp. 238-245
Author(s):  
Dagmara Sowińska ◽  
Alicja Pogorzelska ◽  
Marlena Rakicka ◽  
Justyna Sznura ◽  
Justyna Janowska ◽  
...  
Keyword(s):  
Human Plasma ◽  
Internal Standard ◽  
Hplc Method ◽  
Active Metabolites ◽  
Peak Separation ◽  
Rp Hplc ◽  
Increased Risk ◽  
Relative Standard ◽  
Development And Validation

Background: Atorvastatin (AT) belongs to cholesterol-lowering agents, commonly used in patients with an increased risk of cardiovascular disease. The drug, as well as its hydroxyl metabolites, exhibit pharmacological activity, and their plasma levels may be helpful in the assessment of the therapeutic effectiveness. Objective: Development and validation of a fast and reproducible RP-HPLC method with UV detection for the simultaneous determination of atorvastatin and its active metabolites, para-hydroxy-atorvastatin (p-OH-AT) and ortho-hydroxy-atorvastatin (o-OH-AT) in human plasma. Methods: Optimal conditions of chromatographic separation of the analytes, as well as rosuvastatin, chosen as an internal standard, were studied. The absorbance of the compounds was measured at λ=248 nm. Validation of the method was performed. The usefulness of the method was confirmed for determination of the analytes in plasma of patients treated with the drug. Results: Total peak separation was achieved at LiChrospher 100 RP-18 column with a mobile phase composed of methanol and water (1:1,v:v) and a flow rate of 1.2 ml/min. The method was linear in the ranges of 0.025 - 1.0 μg/ml for AT, o-OH-AT and p-OH-AT. Intra- and inter-assay precision expressed as relative standard deviation was ≤13% for AT, ≤12% for p-OH-AT and ≤11% for o-OH-AT. Intraand inter-day accuracy of the method, expressed as a relative error, was ≤15%. Conclusion: The elaborated HPLC method is specific, repeatable, reproducible, adequately accurate and precise and fulfills the validation requirements for the bioanalytical method. The method was successfully applied for analysis of atorvastatin and its o-hydroxy metabolite in plasma of patients treated with the drug.

scholarly journals Validation and Optimization of a Simple RP-HPLC Method for the Determination of Paracetamol in Human Serum and its Application in a Pharmacokinetic Study with Healthy Bangladeshi Male Volunteers

2015 ◽  
Vol 13 (2) ◽  
pp. 125-131
Author(s):  
Anisa Alam Tanam ◽  
Mohammad Firoz Khan ◽  
Ridwan Bin Rashid ◽  
Md Zakir Sultan ◽  
Mohammad A Rashid
Keyword(s):  
Human Serum ◽  
Pharmacokinetic Study ◽  
Internal Standard ◽  
Immediate Release ◽  
Hplc Method ◽  
Serum Samples ◽  
Limit Of Quantification ◽  
Rp Hplc ◽  
Relative Standard

Acetaminophen (paracetamol) is an analgesic and antipyretic agent with minimum anti-inflammatory properties. In the present study a simple, fast, accurate, precise and reproducible RP-HPLC method has been developed and validated for the quantification of paracetamol in human serum samples using theophylline as internal standard. Protein precipitation with perchloric acid was employed in the extraction of paracetamol and theophylline from biological matrix. The chromatographic separation was accomplished on Phenomenex C18 column with a mobile phase comprising of 0.05 mM sodium sulfate buffer (pH 2.2 ± 0.02 adjusted with phosphoric acid) and acetonitrile at a ratio of 93:7 at a flow rate of 1.0 ml/min. The chromatogram was monitored by UV detection at a wavelength of 254 nm. The method was validated over a linear concentration range of 2-100 ?g/ml and limit of quantification (LOQ) was 1.61 ?g/ml with a correlation coefficient (r2) 0.997. The intra-day and inter-day precision expressed as relative standard deviation were found to be 0.49 - 2.68% and 0.36 - 3.44%, respectively. The average recovery of paracetamol from serum ranged from 99.0 - 106.4%. The method was successfully applied to a pharmacokinetic study after oral administration of immediate release paracetamol tablet (1000 mg) in four healthy Bangladeshi volunteers. The mean Cmax was found to be 11.03 ± 3.21 ?g/ml, which occurred at Tmax of 0.88 ± 0.14 hr. The half life, AUC0-8 and AUC0-? values were found to be 3.09 ± 0.71 hr, 31.06 ± 6.57 hr-?g/ml and 37.92 ± 9.51 hr- ?g/ml, respectively. DOI: http://dx.doi.org/10.3329/dujps.v13i2.21889 Dhaka Univ. J. Pharm. Sci. 13(2): 125-131, 2014 (December)

scholarly journals Comparison of High-Performance Liquid Chromatographic and Microbiological Methods for Determination of Voriconazole Levels in Plasma

2000 ◽  
Vol 44 (5) ◽  
pp. 1209-1213 ◽  
Author(s):  
Sofia Perea ◽  
Gennethel J. Pennick ◽  
Asha Modak ◽  
Annette W. Fothergill ◽  
Deanna A. Sutton ◽  
...  
Keyword(s):  
High Performance ◽  
High Performance Liquid Chromatographic ◽  
Hplc Method ◽  
Pharmacokinetic Studies ◽  
Serum Samples ◽  
Bioassay Method ◽  
Microbiological Methods ◽  
And Control ◽  
Liquid Chromatographic

ABSTRACT A new selective high-performance liquid chromatography (HPLC) method with UV detection for the determination of the investigational triazole voriconazole in human plasma by using acetonitrile precipitation followed by reverse-phase HPLC on a C18column was compared with a simple agar well diffusion bioassay method with Candida kefyr ATCC 46764 as the assay organism. Pooled plasma was used to prepare standard and control samples for both methods. The results of analyses with spiked serum samples (run as unknowns) were concordant by the bioassay and HPLC methods, with expected values being obtained. HPLC demonstrated an improved precision (3.47 versus 12.12%) and accuracy (0.81 versus 1.28%) compared to those of the bioassay method. The range of linearity obtained by both methods (from 0.2 to 10 μg/ml for HPLC and from 0.25 to 20 μg/ml for the bioassay) includes the range of concentrations of voriconazole (from 1.2 to 4.7 μg/ml) which are considered clinically relevant. Although either methodology could be used for the monitoring of patient therapy, the smaller variability observed with HPLC compared to that observed with the bioassay favors the use of HPLC for pharmacokinetic studies.

Determination of olanzapine and desmethylolanzapine in the plasma of schizophrenic patients by means of an improved HPLC method with amperometric detection

2001 ◽  
Vol 54 (3-4) ◽  
pp. 203-207 ◽  
Author(s):  
M. A. Raggi ◽  
R. Mandrioli ◽  
C. Sabbioni ◽  
N. Ghedini ◽  
S. Fanali ◽  
...  
Keyword(s):  
Amperometric Detection ◽  
Hplc Method ◽  
Schizophrenic Patients
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