Development and application of a urine drug concentration method for the evaluation of oral absorption of ibandronate in clinical patients

Bioanalysis ◽  
2019 ◽  
Vol 11 (14) ◽  
pp. 1337-1345
Author(s):  
Jing An ◽  
Ye Jiang ◽  
Yanfang Lu ◽  
Lin Zhang ◽  
Meng Xu ◽  
...  
Keyword(s):  
Vitamin D ◽  
Human Urine ◽  
Drug Concentration ◽  
Oral Absorption ◽  
Liquid Extraction ◽  
Concentration Method ◽  
Liquid Liquid Extraction ◽  
Relative Standard ◽  
Urine Drug ◽  
Urine Matrix

Aim: A urine drug concentration method was developed for the evaluation of oral ibandronte absorption based on the fact that ibandronate is excreted unchanged by the kidneys. Methodology: Ibandronate was isolated from the urine matrix by coprecipitated with 2.5 M CaCl2 and 1 M K2HPO4 in basic conditions. After a liquid–liquid extraction, the analytes were derivatized with trimethylsilydiazomethane prior to detection. Results: The calibration curves exhibited excellent linearity (r > 0.99) between 1 and 250 ng/ml in human urine. Ibandronate was recovered >86.5% with the inter- and intraday relative standard deviations less than 15%. Conclusion: The method is selective, accurate, practical and was successfully applied to study the influence of vitamin D3 on the absorption of ibandronate.

scholarly journals The Development and Validation of a Novel Designer Benzodiazepines Panel by LC–MS-MS

2021 ◽  
Author(s):  
Rebecca A Mastrovito ◽  
Donna M Papsun ◽  
Barry K Logan
Keyword(s):  
Illicit Drug ◽  
Liquid Extraction ◽  
Electrospray Tandem Mass Spectrometry ◽  
Method Performance ◽  
Internal Standards ◽  
Liquid Liquid Extraction ◽  
Relative Standard ◽  
Development And Validation ◽  
Positive Ion ◽  
Designer Benzodiazepines

Abstract Novel illicit benzodiazepines are among the most active areas of new illicit drug manufacture and use. We describe a method for the detection and quantification of etizolam and its metabolite α-hydroxyetizolam, flubromazolam, clonazolam, diclazepam, delorazepam, bromazepam, flubromazepam, phenazepam, flualprazolam, flunitrazolam, and nitrazolam in human whole blood. After addition of internal standards, samples are buffered and extracted using a liquid–liquid extraction. Analysis is performed using positive-ion electrospray tandem mass spectrometry for detection and quantitation. Calibration ranges were established based on the method performance and differed from compound to compound. Replicates at the lowest calibration point for each compound performed within 5% of CV (Coefficient of Variation). The correlation coefficient was >0.990 for all compounds. Relative standard deviation for all compounds was ≤10% of CV and accuracy was  ±10% for both within- and between-run experiments. The maximum average intra- and inter-run imprecision were 5.7%. The maximum average intra- and inter-run imprecision was −8.7%. As part of evaluating the scope for relevancy, samples testing positive in immunoassay but confirmed to be negative in traditional benzodiazepine confirmation method were re-analyzed using this method. The presence of at least one novel benzodiazepine was identified in 70% of these samples. The appearance of these novel “designer” benzodiazepines demonstrates the challenge for toxicology testing and the need for continually updated confirmation methods.

scholarly journals Homogeneous Liquid-Liquid Extraction Method for Selective Separation and Preconcentration of Trace Amounts of Palladium

2009 ◽  
Vol 6 (4) ◽  
pp. 1077-1084 ◽  
Author(s):  
Mohammad Reza Jamali ◽  
Yaghoub Assadi ◽  
Reyhaneh Rahnama Kozani ◽  
Farzaneh Shemirani
Keyword(s):  
Extraction Method ◽  
Limit Of Detection ◽  
Liquid Extraction ◽  
Selective Separation ◽  
Complexing Agent ◽  
Homogeneous Liquid ◽  
Liquid Liquid Extraction ◽  
Relative Standard ◽  
Separation And Preconcentration ◽  
Ternary Component System

A simple and effective homogeneous liquid-liquid extraction method for selective separation, preconcentration and spectrophotometric determination of palladium(II) ion was developed by using a ternary component system (water / tetrabutylammonium ion (TBA+) / chloroform). The phase separation phenomenon occurred by an ion–pair formation of TBA+and perchlorate ion. Thio-Michler’s ketone (TMK), 4, 4ˊ-bis (dimethylamino) thiobenzophenone, was used as a complexing agent. After optimization of complexation and extraction conditions ([TMK]=5.0x10-2mol L-1, [TBA+] = 2.0×10-2mol L-1, [CHCl3] = 60.0 µL, [ClO4-] = 2.5×10-2mol L-1and pH= 3.0), a preconcentration factor 10 was obtained for 10 mL of sample. The analytical curve was linear in the range of 2-100 ng mL-1and the limit of detection was 0.4 ng mL-1. The relative standard deviation was 3.2% (n=10). Accuracy and application of the method was estimated by using test samples of natural and synthetic water spiked with different amounts of palladium(II) ion. The method is very simple and inexpensive.

Determination of Tin in Canned Fruits and Vegetables by Atomic Absorption Spectrometry and Liquid–Liquid Extraction

1994 ◽  
Vol 77 (6) ◽  
pp. 1627-1630 ◽  
Author(s):  
Ana M Martín ◽  
Mercedes Sánchez ◽  
Pedro Espinosa ◽  
Gracia Bagur
Keyword(s):  
Aqueous Phase ◽  
Fruits And Vegetables ◽  
Methyl Ketone ◽  
Absorption Spectrometry ◽  
Liquid Extraction ◽  
Acid Complex ◽  
Liquid Liquid Extraction ◽  
Relative Standard ◽  
Good Agreement

Abstract A method was developed for the determination of tin based on the extraction of its 5,5-methylenedisalicylohydroxamic acid complex with 1.09M isobutyl methyl ketone in tributyl phosphate. After the samples were treated with nitric and hydrochloric acid, the aqueous phase was made to 0.05M in perchloric acid. When the ratio of aqueous phase to organic phase was 4:1 (v/v), the detection limit and the relative standard deviation (n = 7,50 μg tin) were 0.20 μg/mL and 0.9%, respectively. The proposed method was applied to the analysis of tin in canned fruits and vegetables. The results were in good agreement with those obtained by the phenylfluorone method.

scholarly journals COMPARISON OF THREE EXTRACTION METHODS OF ALLOPURINOL IN URIC ACID HERBAL MEDICINE WITH HIGH-PERFORMANCE LIQUID CHROMATOGRAPHY QUANTIFICATION

2021 ◽  
pp. 141-147
Author(s):  
RIMADANI PRATIWI ◽  
RASPATI D. MULYANINGSIH ◽  
NYI M. SAPTARINI
Keyword(s):  
Herbal Medicine ◽  
High Performance ◽  
Solid Phase ◽  
Extraction Methods ◽  
Liquid Extraction ◽  
Filtering Method ◽  
Liquid Liquid Extraction ◽  
Accuracy And Precision ◽  
Relative Standard ◽  
Parameters Of Accuracy

Objective: This study was aimed to understand and determine the effectiveness of allopurinol extraction in herbal medicine from three extraction methods based on parameters of accuracy and precision. Methods: The study consisted of three methods including dissolving and filtering, liquid-liquid extraction, and solid-phase extraction with mixed-mode cation exchanger (SPE-MCX). The procedures were carried out using NaOH and HCl in dissolving and filtering method; methanol, HCl, and ethyl acetate in liquid-liquid extraction; and NH4OH elution solvent in SPE-MCX. Results: The results showed that extraction effectiveness based on accuracy level was the dissolving and filtering method>SPE-MCX>liquid-liquid extraction with % recovery+SD of 91.314+2.903%, 87.533+4.950%, and 54.549+3.517%, respectively. The precision level was the dissolution and filtering method>SPE-MCX>liquid-liquid extraction based on % relative standard deviations (RSD) of 3.18%, 5.226%, and 6.446%, respectively. Conclusion: It can be concluded that the allopurinol extraction method with the highest effectiveness based on accuracy and precision parameters in herbal medicine is the dissolving and filtering method.

Liquid-liquid extraction-assisted SERS-based determination of sulfamethoxazole in spiked human urine

2020 ◽  
Vol 1109 ◽  
pp. 61-68 ◽  
Author(s):  
Natalia E. Markina ◽  
Alexey V. Markin ◽  
Karina Weber ◽  
Jürgen Popp ◽  
Dana Cialla-May
Keyword(s):  
Human Urine ◽  
Liquid Extraction ◽  
Liquid Liquid Extraction ◽  
Spiked Human Urine

scholarly journals Liquid-liquid extraction combined with high performance liquid chromatography-diode array-ultra-violet for simultaneous determination of antineoplastic drugs in plasma

2011 ◽  
Vol 47 (2) ◽  
pp. 363-371 ◽  
Author(s):  
Ananda Lima Sanson ◽  
Suéllen Cristina Rennó Silva ◽  
Matheus Coutinho Gonçalves Martins ◽  
Alexandre Giusti-Paiva ◽  
Patrícia Penido Maia ◽  
...  
Keyword(s):  
High Performance Liquid Chromatography ◽  
Liquid Chromatography ◽  
High Performance ◽  
Liquid Extraction ◽  
Therapeutic Drug ◽  
Diode Array ◽  
Antineoplastic Drugs ◽  
Liquid Liquid Extraction ◽  
Relative Standard

A liquid-liquid extraction (LLE) combined with high-performance liquid chromatography-diode array detection method for simultaneous analysis of four chemically and structurally different antineoplastic drugs (cyclophosphamide, doxorubicin, 5-fluorouracil and ifosfamide) was developed. The assay was performed by isocratic elution, with a C18 column (5 µm, 250 x 4.6 mm) and mobile phase constituted by water pH 4.0- acetonitrile-methanol (68:19:13, v/v/v), which allowed satisfactory separation of the compounds of interest. LLE, with ethyl acetate, was used for sample clean-up with recoveries ranging from 60 to 98%. The linear ranges were from 0.5 to 100 µg mL-1, for doxorubicin and 1 to 100 µg mL-1, for the other compounds. The relative standard deviations ranged from 5.5 to 17.7%. This method is a fast and simple alternative that can be used, simultaneously, for the determination of the four drugs in plasma, with a range enabling quantification of the drugs in pharmacokinetics, bioequivalence and therapeutic drug-monitoring studies.

scholarly journals Stir bar-sorptive extraction, solid phase extraction and liquid-liquid extraction for levetiracetam determination in human plasma: comparing recovery rates

2015 ◽  
Vol 51 (2) ◽  
pp. 393-401 ◽  
Author(s):  
Priscila Freitas-Lima ◽  
Flavia Isaura Santi Ferreira ◽  
Carlo Bertucci ◽  
Veriano Alexandre Júnior ◽  
Sônia Aparecida Carvalho Dreossi ◽  
...  
Keyword(s):  
Solid Phase Extraction ◽  
Solid Phase ◽  
Liquid Extraction ◽  
Stir Bar Sorptive Extraction ◽  
Therapeutic Drug ◽  
Phase Extraction ◽  
Recovery Rates ◽  
Sorptive Extraction ◽  
Liquid Liquid Extraction ◽  
Relative Standard

<p>Levetiracetam (LEV), an antiepileptic drug (AED) with favorable pharmacokinetic profile, is increasingly being used in clinical practice, although information on its metabolism and disposition are still being generated. Therefore a simple, robust and fast liquid-liquid extraction (LLE) followed by high-performance liquid chromatography method is described that could be used for both pharmacokinetic and therapeutic drug monitoring (TDM) purposes. Moreover, recovery rates of LEV in plasma were compared among LLE, stir bar-sorptive extraction (SBSE), and solid-phase extraction (SPE). Solvent extraction with dichloromethane yielded a plasma residue free from usual interferences such as commonly co-prescribed AEDs, and recoveries around 90% (LLE), 60% (SPE) and 10% (SBSE). Separation was obtained using reverse phase Select B column with ultraviolet detection (235 nm). Mobile phase consisted of methanol:sodium acetate buffer 0.125 M pH 4.4 (20:80, v/v). The method was linear over a range of 2.8-220.0 µg mL<sup>-1</sup>. The intra- and inter-assay precision and accuracy were studied at three concentrations; relative standard deviation was less than 10%. The limit of quantification was 2.8 µg mL<sup>-1</sup>. This robust method was successfully applied to analyze plasma samples from patients with epilepsy and therefore might be used for pharmacokinetic and TDM purposes.</p>

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