Fast Method for the Determination of Residual Solvents in Radiopharmaceutical Products

2017 ◽  
Vol 68 (4) ◽  
pp. 666-670 ◽  
Author(s):  
Mirela Mihon ◽  
Catalin Stelian Tuta ◽  
Alina Catrinel Ion ◽  
Dana Niculae ◽  
Vasile Lavric
Keyword(s):  
Gas Chromatography ◽  
Control Method ◽  
Limit Of Detection ◽  
The Body ◽  
Biologically Active ◽  
Injection Technique ◽  
Fast Method ◽  
Residual Solvent ◽  
Residual Solvents

The aim of this work was the development and validation of a fast analytical method to determine the residual solvents content in radiopharmaceuticals such as: 18F-Fluorodeoxyglucose (18F-FDG), 18F-Fluoroestradiol (18F-FES), 18F-Fluorothymidine (18F-FLT),18F-Fluoromisonidazole (18F-FMISO). Radiopharmaceuticals are radioactive preparations for medical purposes used in nuclear medicine as tracers in diagnostic imaging and treatment of certain diseases. Positron Emission Tomography (PET) is a medical imaging technique that consists in introducing into the body of a small amount of a biologically active chemical compound labelled with a short lived positron-emitting radioisotope (18F, 11C, 68Ga). Residual solvents are critical impurities in radiopharmaceuticals that can affect labelling, stability and physicochemical properties of drugs. Therefore, the determination of these solvents is essential for quality control of radiopharmaceuticals. Validation of the control method for residual solvents by gas chromatography is referred by the European Pharmacopoeia using a special injection technique (head space). The parameters of the method, which comply with International Conference on Harmonization guidelines, are: accuracy, precision, linearity, limit of detection, limit of quantification and robustness. The proposed method (direct gas chromatography injection) proved to be linear, precise, accurate and robust. Good linearity was achieved for all the solvents and correlation coefficients (R2) for each residual solvent were found more than 0.99.

Method Development And Validation For Determination Of Residual Solvents In Racecadotril By Gas Chromatography

2020 ◽  
Vol 16 ◽  
Author(s):  
Sirisha Reddy Sattinena ◽  
Alex Joseph ◽  
Subham Das ◽  
B Chaitainya ◽  
Subba Rao
Keyword(s):  
Gas Chromatography ◽  
Simultaneous Determination ◽  
Chromatographic Method ◽  
Isopropyl Alcohol ◽  
Limit Of Detection ◽  
Active Pharmaceutical Ingredients ◽  
Residual Solvents ◽  
Pharmaceutical Ingredients ◽  
Gas Chromatographic Method

Background: Presence of residual solvents in pharmaceuticals can be a potential risk factor to human health because of its toxicity. Gas chromatography used for its excellent separation abilities and lower limit of detection. Racecadotril, an antidiarrheal drug, reported having four residual solvents, namely n-Hexane, isopropyl alcohol, toluene and dimethylformamide. Estimation the amount of these solvents in active pharmaceutical ingredients to ensure that they are within the permissible limits as per ICH guidelines necessary. <p> Objective: To develop and validate a new, simple and sensitive gas chromatographic method for simultaneous determination of n-Hexane, isopropyl alcohol, toluene and dimethylformamide in racecadotril. <p> Method: The residual solvents of racecadotril estimated using a gas chromatographic method by direct injection using FID as a detector. This method employed a 30-meter long DB-FFAP nitroterephthalic-acid-modified polyethene glycol column with 0.53 mm in inner diameter and 1 μm film thickness. The separation achieved using nitrogen as the carrier gas at a flow rate of 2.8 mL/min using a split ratio of 1:10. <p> Results: The peak shape for all the residual solvents from racecadotril was symmetric with excellent resolution eluting at reasonable retention time. The limit of detection of n-Hexane, isopropyl alcohol, Toluene and dimethylformamide found to be 6, 27, 14 and 42 ppm respectively. The developed method exhibited excellent linearity for each residual solvents in the range studied. <p> Conclusion: The developed gas chromatographic method is simple, specific, precise, accurate and sensitive. Hence, the method can be successfully used in the pharmaceutical companies and research laboratories for simultaneous determination of residual solvents in racecadotril active pharmaceutical ingredients.

scholarly journals Method development and validation for the determination of residual solvents in quinabut API by using gas chromatography. Message 2

Pharmacia ◽  
2021 ◽  
Vol 68 (1) ◽  
pp. 53-59
Author(s):  
Оlena Golembiovska ◽  
Oleksii Voskoboinik ◽  
Galina Berest ◽  
Sergiy Kovalenko ◽  
Liliya Logoyda
Keyword(s):  
Gas Chromatography ◽  
Method Development ◽  
Limit Of Detection ◽  
Accurate Method ◽  
Chromatography Method ◽  
Synthetic Process ◽  
Residual Solvent ◽  
Residual Solvents ◽  
All Solutions ◽  
Limit Of Quantitation

Aim. The aim of study was to develop and validate a simple, precise and accurate method using gas chromatography for analysis of residual solvents – acetone and 2-propanol – in quinabut API. Materials and methods. All experiments were performed on a gas chromatographic system equipped with FID detector (Shimadzu GC System) using the DB-624 (30 m × 0.32 mm ID, 3.0 μm film sickness) column as stationary phase. Nitrogen was used as carrier gas with flow rate 7.5 mL/ min. Split ratio was 1:5, injector temperature was 140 °C, detector temperature was 250 °C, oven temperature was programmed from 40 °C (2 min) to 50 °C at 1 °C/min and then increased at a rate of 15 °C/min up to 215 °C; and maintained for 2 min. All solutions were prepared using water as diluent. Results. This proposed method is assessed for separation of residual solvent from quinabut with quantification. The obtained results are compared with the corresponding specified limits of ICH standard guidelines. The method validation was done by evaluating specificity, limit of detection (LOD) and limit of quantitation (LOQ), linearity, accuracy, repeatability, ruggedness, system suitability and method precision of residual solvents as indicated in the ICH harmonized tripartite guideline. The separation between acetone and 2-propanol peaks is 2.07. Hence method was found to be specific. The linear relationship evaluated across range of 15 to 180% for acetone and 2-propanol of ICH specified limit of residual solvents. The graphs of theoretical concentration versus obtained concentration are linear and the regression coefficients ‘R’ for residual solvents were more than 0.9968. The values of LOD and LOQ were much less than the lower limit of the concentration range and cannot affect the accuracy of the test. The technique was characterized by high intra-laboratory accuracy at concentrations close to the nominal acetone and 2-propanol concentration. All solutions were stable in water for at least 1 hour when stored at room temperature. Conclusion. A simple, specific, accurate, precise and rugged gas chromatography method was developed and validated for the quantification of residual solvents present in quinabut API through an understanding of the synthetic process, nature of solvents and nature of stationary phases of columns. The residual solvents acetone and 2-propanol were determined.

scholarly journals An Improved Methodology for Determination of Fluorine in Biological Samples Using High-Resolution Molecular Absorption Spectrometry via Gallium Fluorine Formation in a Graphite Furnace

2021 ◽  
Vol 11 (12) ◽  
pp. 5493
Author(s):  
Andrzej Gawor ◽  
Andrii Tupys ◽  
Anna Ruszczyńska ◽  
Ewa Bulska
Keyword(s):  
High Resolution ◽  
Limit Of Detection ◽  
Graphite Furnace ◽  
Absorption Spectrometry ◽  
Biological Tissues ◽  
Biologically Active ◽  
Molecular Absorption ◽  
Biological Origin ◽  
Molecular Absorption Spectrometry

Nowadays growing attention is paid to the control of fluorine content in samples of biological origin as it is present in the form of various biologically active organic compounds. Due to the chemically-rich matrix of biological tissues, the determination of fluorine becomes a very difficult task. Furthermore, a required complex sample preparation procedure makes the determination of the low contents of F by ion chromatography UV-Vis or ion-selective electrodes not possible. High-resolution continuum source graphite furnace molecular absorption spectrometry (HR-CS GF MAS) seems to be the best option for this purpose due to its high robustness to matrix interferences, especially in the presence of carefully selected modifiers. In this work the possibility of quantitative F determination in water and animal tissues was examined by measuring the molecular absorption of gallium monofluoride (GaF) at 211.248 nm with the use of a commercially available HR-CS GF MAS system. Experimental conditions for the sensitive and precise determination of fluorine were optimized, including the time/temperature program as well as addition of gallium and modifier mixture in combined mode. Under these conditions the fluoride present in the sample was stabilized up to 600 °C, and the optimum vaporization temperature for GaF was 1540 °C. Palladium and zirconium deposited onto the graphite surface served as solid modifiers; sodium acetate and ruthenium modifiers were added directly to the sample. The limit of detection and the characteristic mass of the method were 0.43 μg/L and 8.7 pg, respectively. The proposed procedure was validated by the use of certified reference materials (CRMs) of lake water and animal tissue; the acceptable recovery was obtained, proving that it can be applied for samples with a similar matrix.

Method of Validation for Residual Solvents in Bisoprolol Fumarate by GC Technique

2021 ◽  
pp. 147-155
Author(s):  
Sandip A Telavane ◽  
Seema Kothari ◽  
Manohar V. Lokhande
Keyword(s):  
Limit Of Detection ◽  
Chromatographic Technique ◽  
Range Limit ◽  
Column Temperature ◽  
Residual Solvent ◽  
Residual Solvents ◽  
Validation Parameters ◽  
Limit Of Quantitation ◽  
Chromatographic Condition ◽  
Methylene Dichloride

Validation is important technique for detection, progress and estimation of drugs for pharmaceutical analysis. Aim of this article was to check the progress and validation of the method employed for the Residual Solvents in Bisoprolol Fumarate by Gas Chromatographic technique. The objective of this protocol is to validate a GC method of analysis for detection and Quantification of Residual Solvents Methanol, Acetone and Methylene dichloride in Bisoprolol Fumarate. In the pharmaceutical industry, validation policy is more important for documented of validation, types of validation and validation policy. The method was developed accurately and validation parameters are explained. Chromatographic condition was GC- 2014, gas chromatograph equipped with FID detector, column: 30 m x 0.32 mm ID x 1.8 µm DB - 624 capillary column or equivalent and column temperature was 45°C (hold 7 minutes) to 250°C @ 40°C/minutes, hold at 250°C for 3 minutes. The parameters such as Accuracy, Specificity, Precision, Linearity and Range, Limit of detection (LOD), Limit of quantitation (LOQ), ruggedness, robustness and system suitability testing with residual solvent such as Methanol, Acetone and methylene dichloride. All validation parameters are used in the routine and stability analysis.

Determination of multiple organochlorine pesticide residues in shrimp using modified QuEChERS extraction and gas chromatography

2018 ◽  
Vol 16 (1) ◽  
pp. 81-93
Author(s):  
MDH Prodhan ◽  
SN Alam
Keyword(s):  
Gas Chromatography ◽  
Organochlorine Pesticide ◽  
Pesticide Residues ◽  
Limit Of Detection ◽  
Residue Analysis ◽  
Limit Of Quantification ◽  
Modified Quechers ◽  
Endosulfan Sulphate ◽  
Organochlorine Pesticide Residues

Determination of organochlorine pesticide residues in shrimp is very important to ensure the consumer’s safety and to fulfill the importer’s demand. Therefore, a simple and efficient multiple organochlorine pesticide residues analytical method using quick, easy, cheap, effective, rugged and safe (QuEChERS) extraction technique and Gas Chromatography coupled with Electron Capture Detector (ECD) has been developed and validated for the determination of 19 organochlorine pesticides (α- BHC, δ- BHC, β- BHC, γ- BHC, Heptachlor, Aldrin, Heptachlor Epoxide, γ- Chlordane, α- Chlordane, α- Endosulfan, 4,4 DDE, Dieldrin, Endrin, 4,4 DDD, β- Endosulfan, 4,4 DDT, Endosulfan sulphate, Methoxychlor, and Endrin Ketone) in shrimp. The method was validated by evaluating the accuracy, precision, linearity, limit of detection (LOD) and limit of quantification (LOQ). The average recoveries of the selected pesticides ranged from 84% to 106% with RSDr ≤ 14% in four fortification levels of 0.05, 0.1, 0.2 and 0.3 mg kg-1. The linearity was ≥ 0.996 for all of the selected pesticides with matrix matched calibration standards. The LOD ranged from 0.003 to 0.009 mg kg-1 and the LOQ was 0.05 mg kg-1. This method was applied successfully for the residue analysis of 40 shrimp samples collected from different regions in Bangladesh.SAARC J. Agri., 16(1): 81-93 (2018)

Reliable Method for the Determination of Food Additive by Capillary Electrophoresis Using a Microvolume of Foodstuffs

2011 ◽  
Vol 361-363 ◽  
pp. 1486-1489
Author(s):  
Qian Xiang ◽  
Ying Gao
Keyword(s):  
Capillary Electrophoresis ◽  
Reliable Method ◽  
Lower Cost ◽  
Limit Of Detection ◽  
Food Additive ◽  
Fast Method ◽  
Optimum Conditions ◽  
Applied Potential ◽  
Minimal Sample

A fast method for the separation and determination of the food additive propyl gallate has been established by using capillary electrophoresis. The effects of several factors such as the applied potential and detection running buffer were investigated in order to obtain the optimum conditions, and the assay results were satisfactory. The limit of detection for the analyte was 10-6 mol/L. This approach has remarkable advantages with respect to other methodologies involving separations and electrochemical detection including minimal sample consumption, higher analysis speed and lower cost. In order to demonstrate the capabilitiy of the method, the determination of additive in a commercial food sample is also presented.

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