Development and Validation of a Method for the Detection and Quantification of Antidepressants and Antipsychotics in Bone Samples by GC–MS

2020 ◽  
Author(s):  
Antonino Laudani ◽  
Deborah Sangregorio ◽  
Pietro Zuccarello ◽  
Teresa Licciardello ◽  
Stephanie Grasso ◽  
...  
Keyword(s):  
Bone Marrow ◽  
Analytical Method ◽  
Forensic Toxicology ◽  
Selected Ion Monitoring ◽  
Method Performance ◽  
Matrix Interferences ◽  
Potential Alternative ◽  
Development And Validation ◽  
Method Of Extraction ◽  
Human Autopsy

Abstract Bone marrow is the tissue contained inside the bones and can be considered one of the potential alternative tissues in forensic toxicology. This matrix could be particularly useful in those cases where the routine sample is not available due to an advanced state of decomposition or skeletonization of the corpse. The aim of this study was to develop, validate and apply an analytical method of extraction and analysis of different antidepressants and antipsychotics, commonly used in therapy, from spiked pig ribs. Pig ribs, each of 5 g and 5 cm long, were spiked at 3 concentration levels (100, 200 and 500 ng/g). For each concentration, 10 pig ribs were prepared. The method involves the leaching by ethanol at different pHs of nine drugs from the inside of ribs, in particular from the bone marrow, without the fragmentation of bone tissue. Following a liquid–liquid purification and extraction, analysis was performed by gas chromatography coupled with mass spectrometry in selected ion monitoring mode. For method validation was assessed linearity, sensitivity, precision and accuracy, matrix interferences and, finally, carryover. Analytical method performance was acceptable respect to acceptance criteria for validation. No matrix interferences were detected; for this reason, it is possible to affirm that this method has a good selectivity. Moreover, the method was not affected by carryover. Considering that the study conducted on pig ribs has given encouraging results, it can be assumed that this method can be used in forensic toxicological protocols (human autopsy cases) as alternative to classic procedures.

scholarly journals Quality by Design Approach for an Orally Disintegrating Tablet Analytical Method Validation

2018 ◽  
Vol 10 (01) ◽  
Author(s):  
G. Demire ◽  
D. Saray ◽  
B. Yaman, A. Turkyilmaz Yaman ◽  
A. Turkyilmaz
Keyword(s):  
Analytical Method ◽  
Method Development ◽  
Quality By Design ◽  
Hplc Method ◽  
Method Performance ◽  
Analytical Method Validation ◽  
Orally Disintegrating Tablet ◽  
Method Development And Validation ◽  
Quality By Design Approach ◽  
Development And Validation

Quality by Design (QbD) is well established in the pharmaceutical industry for pharmaceutical development and manufacturing processes. The knowledge obtained during development may support the establishment of a design space and determines suitable process controls. This same QbD principle has been applied to the development of analytical methods and is termed “Analytical Quality by Design” (AQbD). Analogous to process QbD, the outcome of AQbD is well understood, fit for purpose, and robust method that consistently delivers the intended performance throughout its life cycle. The present work is aimed to develop an AQbD approach to analytical method development and validation based of Tadalafil and its impurities by the NP-HPLC method. The other objective of this work is to establish an in-depth understanding of the method and build in the quality during the method development to ensure optimum method performance over the lifetime of the product.

scholarly journals DEVELOPMENT AND VALIDATION OF AN ANALYTICAL METHOD FOR CONDENSED TANNIN EXTRACTS OBTAINED FROM THE BARK OF FOUR TREE SPECIES USING HPLC

Wood Research ◽  
2021 ◽  
Vol 66 (2) ◽  
pp. 171-182
Author(s):  
Faustino Ruiz Aquino ◽  
Rossy Feria Reyes ◽  
José Guadalupe Rutiaga Quiñones ◽  
Wenceslao Santiago García ◽  
Mario Ernesto Suárez Mota ◽  
...  
Keyword(s):  
Infrared Spectroscopy ◽  
Analytical Method ◽  
Tree Species ◽  
Condensed Tannins ◽  
High Performance ◽  
Condensed Tannin ◽  
Hydroxyl Group ◽  
Aromatic Esters ◽  
Development And Validation ◽  
Method Of Extraction

Herein, we evaluated the content of condensed tannins present in the bark of four tree species that are Quercus laurina Humb. & Bonpl., Quercus crassifolia Humb. & Bonpl., Arbutus xalapensis Kunth, and Prunus serotina Ehrn. An analytical method using high-performance liquid chromatography (HPLC) for condensed tannin extracts was developed and validated. Also, the aqueous extracts were analyzed by Fourier transform infrared spectroscopy (FTIR). Based on the Stiasny number, A. xalapensis, and Q. laurina represent an important source of condensed tannins, which may be subject to exploitation. Using infrared spectroscopy, it was observed that tannins do not show an important signal of carbonyl groups (aromatic esters) with respect to high purity catechin. Furthermore, the band of the hydroxyl group is less pronounced in tannins, because various hydroxyl are interacting with each other. However, it can be seen that the method of extraction of wood tannins developed in this work, presents satisfactory results.

scholarly journals Lipemia in the Plasma Sample Affects Fentanyl Measurements by Means of HPLC-MS2 after Liquid-Liquid Extraction

Molecules ◽  
2021 ◽  
Vol 26 (15) ◽  
pp. 4514
Author(s):  
Marta Tikhomirov ◽  
Tomasz Śniegocki ◽  
Błażej Poźniak
Keyword(s):  
Forensic Toxicology ◽  
Liquid Extraction ◽  
Rabbit Plasma ◽  
Chromatography Method ◽  
Method Performance ◽  
Liquid Liquid Extraction ◽  
Normal Plasma ◽  
Validation Procedure ◽  
Liquid Chromatography Method ◽  
The Impact

Examination of fentanyl levels is frequently performed in certain scientific evaluations and forensic toxicology. It often involves the collection of very variable blood samples, including lipemic plasma or serum. To date, many works have reported the methods for fentanyl detection, but none of them have provided information about the impact on the assay performance caused by an excessive amount of lipids. This aspect may be, however, very important for highly lipophilic drugs like fentanyl. To address this issue, we developed the liquid chromatography method with mass spectrometry detection and utilized it to investigate the impact of lipids presence in rabbit plasma on the analytical method performance and validation. The validation procedure, conducted for normal plasma and lipemic plasma separately, resulted in good selectivity, sensitivity and linearity. The limits of detection and quantification were comparable between the two matrices, being slightly lower in normal plasma (0.005 and 0.015 µg/L) than in lipemic plasma (0.008 and 0.020 µg/L). Liquid–liquid extraction provided a low matrix effect regardless of the lipid levels in the samples (<10%), but pronounced differences were found in the recovery and accuracy. In the normal plasma, this parameter was stable and high (around 100%), but in the lipemic matrix, much more variable and less efficient results were obtained. Nevertheless, this difference had no impact on repeatability and reproducibility. In the present work, we provided reliable, convenient and sensitive method for fentanyl detection in the normal and lipemic rabbit plasma. However, construction of two separate validation curves was necessary to provide adequate results since the liquid-liquid extraction was utilized. Therefore, special attention should be paid during fentanyl quantification that involves lipemic plasma samples purified by this technique.

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 &gt;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.

Development and Validation of an HPLC Method for Determination of Spirotetramat and Spirotetramat cis enol in Various Vegetables and Soil

2013 ◽  
Vol 96 (3) ◽  
pp. 670-675 ◽  
Author(s):  
Balwinder Singh ◽  
Kousik Mandal ◽  
Sanjay K Sahoo ◽  
Urvashi Bhardwaj ◽  
Raminderjit Singh Battu
Keyword(s):  
Analytical Method ◽  
Anhydrous Sodium Sulfate ◽  
Hplc Method ◽  
Array Detector ◽  
Photodiode Array Detector ◽  
Photodiode Array ◽  
Precision And Accuracy ◽  
Hplc Grade Acetonitrile ◽  
Development And Validation

Abstract An easy and simple analytical method was standardized and validated for the estimation of residues of spirotetramat and its metabolite spirotetramat cis enol in various substrates: okra fruits, brinjal leaves and fruits, green chili, red chili, and soil. The samples were extracted with acetonitrile, diluted with brine solution, partitioned into dichloromethane, dried over anhydrous sodium sulfate, and cleaned up by treatment with activated charcoal powder. Final clear extracts were concentrated under vacuum and reconstituted with HPLC grade acetonitrile. Residues were estimated using HPLC with a photodiode array detector and a C18 column, and confirmed by HPTLC. Acetonitrile was used as the mobile phase at 0.4 mL/min. Both spirotetramat and spirotetramat cis enol presented distinct peak at retention times of 8.518 and 7.598 min, respectively. Consistent recoveries ranging from 82 to 97% for spirotetramat and spirotetramat cis enol were observed when samples were spiked at 1.00 to 0.03 mg/kg levels. The LOQ of the method was found to be 0.03 mg/kg. The analytical method was validated in terms of parameters, including selectivity, linearity, precision, and accuracy.

Development and Validation of a Green Analytical Method for the Determination of Norfloxacin in Raw Material by FTIR Spectrophotometry

2016 ◽  
Vol 99 (6) ◽  
pp. 1533-1536 ◽  
Author(s):  
Jéssica Sayuri Hisano Natori ◽  
Eliane Gandolpho Tótoli ◽  
Hérida Regina Nunes Salgado
Keyword(s):  
Urinary Tract ◽  
Organic Solvents ◽  
Analytical Method ◽  
Environmentally Friendly ◽  
Raw Material ◽  
Waste Generation ◽  
Ftir Spectrophotometry ◽  
Tract Infections ◽  
Development And Validation

Abstract Norfloxacin is a broad-spectrum antimicrobial agent, widely used in humans and animals for the treatment of urinary tract infections. It is a second-generation fluoroquinolone. Several analytical methods to analyze norfloxacin have been described in the literature. However, most of them are complex and require the use of large amounts of organic solvents. This paper describes the development and validation of a green analytical method for the determination of norfloxacin in raw material by FTIR spectrophotometry. This method does not require the use of organic solvents, minimizing waste generation in the process and its environmental impacts. The development of methods that promote the reduction, prevention, or elimination of waste generation has become highly attractive to the pharmaceutical industry because of the growing demand from civil society and government authorities for environmentally friendly products and services. The FTIR spectrophotometry method was validated according to International Conference on Harmonization guidelines, showing adequate linearity (r = 0.9936), precision, accuracy, and robustness. This validated method can be used as an environmentally friendly alternative for the quantification of norfloxacin in raw material in QC routine analysis.

Development and Validation of an Analytical Method Readily Applicable for Quality Control of Tabebuia impetiginosa (Taheebo) Ethanolic Extract

2018 ◽  
Vol 101 (3) ◽  
pp. 695-700 ◽  
Author(s):  
Yan Jin ◽  
Kyung Min Jeong ◽  
Jeongmi Lee ◽  
Jing Zhao ◽  
Su-Young Choi ◽  
...  
Keyword(s):  
Quality Control ◽  
Analytical Method ◽  
Ethanolic Extract ◽  
Development And Validation

scholarly journals Oxcarbazepine: validation and application of an analytical method

2010 ◽  
Vol 46 (2) ◽  
pp. 265-272 ◽  
Author(s):  
Paula Cristina Rezende Enéas ◽  
Renata Barbosa de Oliveira ◽  
Gerson Antônio Pianetti
Keyword(s):  
Spectrophotometric Method ◽  
Analytical Method ◽  
Disintegration Time ◽  
International Conference ◽  
Pharmacopoeial Monograph ◽  
Development And Validation ◽  
Excipient Compatibility

Oxcarbazepine (OXC) is an important anticonvulsant and mood stabilizing drug. A pharmacopoeial monograph for OXC is not yet available and therefore the development and validation of a new analytical method for quantification of this drug is essential. In the present study, a UV spectrophotometric method for the determination of OXC was developed. The various parameters, such as linearity, precision, accuracy and specificity, were studied according to International Conference on Harmonization Guidelines. Batches of 150 mg OXC capsules were prepared and analyzed using the validated UV method. The formulations were also evaluated for parameters including drug-excipient compatibility, flowability, uniformity of weight, disintegration time, assay, uniformity of content and the amount of drug dissolved during the first hour.

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