Method Evaluation Computer Program for Quantitative Analysis of PBBs and PBDEs in Plastics

2010 ◽  
Vol 36 ◽  
pp. 337-343
Author(s):  
Punnee Sittidech ◽  
Manop Sittidech
Keyword(s):  
Quantitative Analysis ◽  
Computer Program ◽  
Analytical Method ◽  
Limit Of Detection ◽  
Diphenyl Ether ◽  
Research Work ◽  
Test Method ◽  
Gas Chromatography Mass Spectrometry ◽  
Polybrominated Biphenyls ◽  
Relative Standard

Polybrominated biphenyls (PBBs) and polybrominated biphenyl ethers (PBDEs) are substances used in electrical and electronic products. They are restricted substances due to their potential risk to human health and the environment. In this research work, a test method was evaluated for the quantitative analysis of polybrominated diphenyl ethers (PBDEs) and polybrominated biphenyls (PBBs) in acrylonitrile-butadiene–styrene (ABS) plastic and polyethylene materials, based on solvent extraction of a plastic sample with soxhlet extraction techniques and detection by gas chromatography/mass spectrometry. We have also developed a computer program for checking the suitability of the analytical method by evaluating validation characteristics, including accuracy, precision, specificity/selectivity, limit of detection (LOD), limit of quantification (LOQ), linearity, range and sensitivity. The computer program was successfully applied for evaluation of the analytical method for prohibited PBBs and PBDEs in plastics. Graphical charts for the evaluation of the analytical method are presented along with their values, and researchers can get insight into evaluating several parameters together. It was found that the analytical method was able to quantify monobrominated - decabrominated biphenyl and monobrominated diphenyl ether–nonabrominated diphenyl ether between 100-1750 mg/kg and decabrominated diphenyl ether between 100–8,000 mg/kg. In addition, ERM-EC590 Polyethylene certified reference material from the Institute for Reference Materials and Measurements (IRMM) was used to validate the analytical method for PBBs and PBDEs in plastics. The obtained accuracy and precision indicate that the method successfully meets the required accuracy expressed as % recovery (70-130%) and the required precision expressed as percentage relative standard deviation (less than 20% RSD) of the IEC 62321:2008 international standard method.

scholarly journals Development and Validation of an Analytical Method for Quantitation of Sulfolane in Rat and Mouse Plasma by GC–MS

2019 ◽  
Vol 43 (6) ◽  
pp. 477-481 ◽  
Author(s):  
Melanie A Rehder Silinski ◽  
Teruyo Uenoyama ◽  
Stephen D Cooper ◽  
Reshan A Fernando ◽  
Veronica G Robinson ◽  
...  
Keyword(s):  
Analytical Method ◽  
Limit Of Detection ◽  
Rat Plasma ◽  
Oil Refining ◽  
Gas Chromatography Mass Spectrometry ◽  
Sprague Dawley ◽  
Mouse Plasma ◽  
Sd Rat ◽  
Relative Standard ◽  
Development And Validation

AbstractSulfolane is an industrial solvent commonly used for extraction of aromatic hydrocarbons in the oil refining process, as well in the purification of natural gas. Its wide use and high solubility in water has led to contamination of groundwater. The objective of this work was to develop and validate an analytical method to quantitate sulfolane in rodent plasma in support of the National Toxicology Program toxicology and toxicokinetic studies of sulfolane. The method uses extraction of plasma with ethyl acetate and analysis by gas chromatography–mass spectrometry with electron ionization. The method was validated in male Sprague Dawley (SD) rat plasma over the concentration range of 20–100,000 ng/mL. The method was linear (r ≥ 0.99), accurate (mean relative error (RE) ≤ ±5.1%) and precise (relative standard deviation (RSD) ≤ 2.9%). The absolute recovery was ≥74%. The limit of detection was 0.516 ng/mL. Standards as high as ~2.5 mg/mL could be successfully diluted into the calibration range (mean %RE ≤ ±4.5; %RSD ≤ 4.6). Extracted samples were stable for at least 3 days at ambient and refrigerated temperatures, and freeze/thaw stability in matrix was demonstrated after three cycles over 3 days (calculated concentrations within 90.8–102% of Day 0 concentrations). Sulfolane was stable in frozen plasma for at least 75 days at −80°C (calculated concentrations within 93.0–98.1% of Day 0 concentrations). Matrix evaluation was performed for sulfolane in female SD rat plasma and male and female B6C3F1 mouse plasma (mean %RE ≤ ±4.9; %RSD ≤ 3.3). These data demonstrate that the method is suitable for determination of sulfolane in rodent plasma.

Comprehensive Analysis of Volatile Compounds in Mouthpiece Cigarette Adhesive by Coupling Headspace with Gas Chromatography-Mass Spectrometry

2020 ◽  
Author(s):  
Min Wei ◽  
Feng Zheng ◽  
Xuyan Song ◽  
Ran Li ◽  
Xi Pan ◽  
...  
Keyword(s):  
Mass Spectrometry ◽  
Gas Chromatography ◽  
Quantitative Analysis ◽  
Volatile Compounds ◽  
Analytical Method ◽  
Gas Chromatography Mass Spectrometry ◽  
Qualitative And Quantitative Analysis ◽  
Qualitative And Quantitative ◽  
Chromatography Mass Spectrometry ◽  
Relative Standard

Abstract Background Some volatile compounds in mouthpiece cigarette adhesive emit irritating odors and affect the taste of smoking cigarettes. Therefore, it is necessary to monitor the volatile compounds in mouthpiece cigarette adhesive. Objectives A rapid and simple analytical method of volatile compounds in mouthpiece cigarette adhesive was established. Methods In this study, headspace (HS) injection coupled with gas chromatography-mass spectrometry (GC-MS) was utilized for qualitative and quantitative analysis. Initially, the volatile compounds in mouthpiece cigarette adhesives were detected by HS-GC-MS, followed by spectrum library retrieval. The detected compounds with the similarity to spectrum library of more than 85% were further identified by comparing the retention time and mass spectra of the detected volatile compounds and those of the corresponding standard samples. The quantitative analysis of 9 identified volatile compounds was performed. Results Eleven volatile compounds in the mouthpiece cigarette adhesive were accurately identified. The quantitative analytical method of 9 volatile compounds in mouthpiece cigarette adhesive was validated to have good linearities (R2 > 0.9932) within the range of 20–5000 ng/g. The detection limits of 9 compounds were within the range of 3.1–147.7 ng/g. The intra- and inter-day relative standard deviations (RSDs) were less than 19.8%. The recoveries of these 9 compounds spiked into mouthpiece cigarette adhesive were from 68.1% to 108.3%. Conclusions The proposed method is rapid, simple, and accurate for qualitative and quantitative analysis of volatile compounds in the mouthpiece cigarette adhesive. Highlights The developed analytical method is expected to be used to monitor volatile compounds in various adhesives.

scholarly journals Quantitative Characteristics of Toxic Compounds According to the Solvent Type

2019 ◽  
Vol 2019 ◽  
pp. 1-9
Author(s):  
Young-Ji An ◽  
Seong-Jin Choi ◽  
Yong-Hyun Kim ◽  
Kyuhong Lee
Keyword(s):  
Quantitative Analysis ◽  
Analytical Data ◽  
Gas Chromatography Mass Spectrometry ◽  
Toxic Compounds ◽  
Solvent Type ◽  
Target Analytes ◽  
Relative Standard ◽  
Rf Values ◽  
Benzene Toluene ◽  
Working Standards

The quantitative analysis of target substances is an important part of assessing the toxicity of diverse materials. Usually, the quantitation of target compounds is conducted by instrumental analysis such as chromatography and capillary electrophoresis. If solvents are used in the pretreatment step of the target analyte quantification, it would be crucial to examine the solvent effect on the quantitative analysis. Therefore, in this study, we assessed the solvent effects using four different solvents (methanol, hexane, phosphate buffered saline (PBS), and dimethyl sulfoxide (DMSO)) and three toxic compounds (benzene, toluene, and methylisothiazolinone (MIT)). Liquid working standards containing the toxic compounds were prepared by dilution with each solvent and analyzed by gas chromatography-mass spectrometry (GC-MS). As a result, we found that the response factor (RF) values of the target analytes were different, depending on the solvent types. In particular, benzene and toluene exhibited their highest RF values (33,674 ng−1 and 78,604 ng−1, respectively) in hexane, while the RF value of MIT was the highest (9,067 ng−1) in PBS. Considering the correlation (R2) and relative standard deviation (RSD) values, all target analytes showed fairly good values (R2 > 0.99 and RSD < 10%) in methanol and DMSO. In contrast, low R2 (0.0562) and high RSD (10.6%) values of MIT were detected in hexane, while benzene and toluene exhibited relatively low R2 and high RSD values in PBS (mean R2 = 0.9892 ± 0.0146 and mean RSD = 13.3 ± 4.1%). Based on these findings, we concluded that the results and reliability of the quantitative analysis change depending on the analyte and solvent types. Therefore, in order to accurately assess the toxicity of target compounds, reliable analytical data should be obtained, preferentially by considering the solvent types.

scholarly journals Preliminary Results on the Use of Leather Chrome Shavings for Air Passive Sampling

2012 ◽  
Vol 2012 ◽  
pp. 1-6 ◽  
Author(s):  
D. Sanjuán-Herráez ◽  
L. Chabaane ◽  
S. Tahiri ◽  
A. Pastor ◽  
M. de la Guardia
Keyword(s):  
Passive Sampling ◽  
Limit Of Detection ◽  
Low Density Polyethylene ◽  
Gas Chromatography Mass Spectrometry ◽  
Low Density ◽  
Relative Standard ◽  
Volatile Organic ◽  
Good Repeatability ◽  
Head Space Gas Chromatography ◽  
Indoor And Outdoor

A new passive sampler based on low-density polyethylene (LDPE) layflat tube filled with chrome shavings from tannery waste residues was evaluated to determine volatile organic compounds (VOCs) in indoor and outdoor areas. VOCs were directly determined by head space-gas chromatography-mass spectrometry (HS-GC-MS) without any pretreatment of the sampler and avoiding the use of solvents. Limit of detection values ranging from 20 to 75 ng sampler−1and good repeatability values were obtained for VOCs under study with relative standard deviation values from 2.8 to 9.6% except for carbon disulfide for which it was 22.5%. The effect of the amount of chrome shavings per sampler was studied and results were compared with those obtained using empty LDPE tubes, to demonstrate the capacity of chrome shavings to adsorb VOCs.

scholarly journals Development and Validation of a Green Analytical Method for the Determination of Aspirin and Domperidone Bulk or Formulation Using UV and HPLC

2020 ◽  
Vol 10 (6) ◽  
pp. 49-56
Author(s):  
Sneha Jagnade ◽  
Pushpendra Soni ◽  
Lavakesh Kumar Omray
Keyword(s):  
Analytical Method ◽  
Method Development ◽  
Limit Of Detection ◽  
Research Work ◽  
Ultra Violet ◽  
Limit Of Quantification ◽  
Intermediate Precision ◽  
Rp Hplc ◽  
Development And Validation

The aim of present study was to investigate the development and validation of a green analytical method for the determination of aspirin and domperidone. Method Development and Validation for Estimation of Domperidone and Aspirin in bulk or formulation by using RP-HPLC. The RP-HPLC method was developed for estimation of Aspirin and Domperidone in synthetic mixture by isocratically using 10 mM KH2PO4: Acetonitrile (20:80) as mobile phase, Prontosil C-18 column (4.6 x 250 mm, 5μparticle size) column as stationary phase and chromatogram was recorded at 231 nm. Then developed method was validated by using various parameters such as, linearity, Range accuracy, precision repeatability, intermediate precision, robustness, limit of detection, limit of quantification. The proposed methods were found to be linear with correlation coefficient close to one. Precision was determined by repeatability, Intermediate precision and reproducibility of the drugs. The robustness of developed method was checked by changing in the deliberate variation in solvent. The result obtained shows the developed methods to be Cost effective, Rapid (Short retention time), Simple, Accurate (the value of SD and % RSD less than 2), Precise and can be successfully employed in the routine analysis of these drugs in bulk drug as well as in tablet dosage form. The Simplicity, Rapidly and Reproducibility of the proposed method completely fulfill the objective of this research work. Keywords: Asprin; Domperidone; HPLC; Ultra Violet; Validation

scholarly journals Effect of Pretreatment on Detection of 37 Pesticide Residues in Chrysanthemum indicum

2021 ◽  
Vol 2021 ◽  
pp. 1-12
Author(s):  
Xiao-Ying Lu ◽  
Yan-Qin Ouyang ◽  
Wei-Ya Zeng ◽  
Cui-Qing Lin ◽  
Lu-Hua Xiao ◽  
...  
Keyword(s):  
Matrix Effect ◽  
Limit Of Detection ◽  
Solid Phase ◽  
Gas Chromatography Mass Spectrometry ◽  
Enhancement Effect ◽  
Matrix Solid Phase Dispersion ◽  
Phase Dispersion ◽  
Chrysanthemum Indicum ◽  
Relative Standard ◽  
Limit Of Quantitation

This study aimed to develop a method, followed by gas chromatography-mass spectrometry, for detecting 37 pesticides in Chrysanthemum indicum (C. indicum) and investigating the decrease in the matrix-induced enhancement effect. The influence of QuEChERS extraction and matrix solid-phase dispersion (MSPD) on the recovery and matrix effect (ME) was compared. extraction and matrix solid-phase dispersion (MSPD) on the recovery and matrix effect (ME) was compared to decrease the ME. The cleanup sorbents, volume and type of solvent, and treatment time were optimized. The accuracy (as recovery), precision (as relative standard deviation, RSD), linearity, limit of quantitation, and limit of detection were determined. The recoveries at the three levels using mixed standard solution ranged between 76% and 120% with RSD ≤15%, and 76% and 120% with RSD ≤11% for MSPD and QuEChERS extraction, respectively. The results suggested that the ME for 21 pesticides was in the range of 80%–120% after MSPD and 15% after QuEChERS extraction. QuEChERS extraction was simpler and faster than MSPD. This methodology was applied in the analysis of 27 C. indicum samples; phorate was most frequently detected (63.0% of the sample).

scholarly journals ANALYTICAL METHOD VALIDATION OF ICP-AES FOR ANALYSIS OF CADMIUM, CHROMIUM, CUPRUM, MANGAN AND NICKEL IN MILK

2019 ◽  
pp. 341-344
Author(s):  
DAVID ALEXANDER ◽  
Abdul Rohman
Keyword(s):  
Heavy Metals ◽  
Analytical Method ◽  
Limit Of Detection ◽  
Official Method ◽  
Fast Method ◽  
Limit Of Quantification ◽  
Milk Products ◽  
Relative Standard ◽  
Validation Parameters

Objective: The aim of this research was to validate inductively coupled plasma-atomic emission spectroscopy (ICP-AES) for quantitative analysis of cadmium (Cd), chromium (Cr), cuprum (Cu), mangan (Mn) and nickel (Ni) in milk products. Methods: The heavy metals in milk were determined using ICP-AES at optimized wavelength. The method was validated by assessing several validation parameters which included linearity and range, accuracy, precision and sensitivity expressed by the limit of detection and limit of quantification. The validated method was then used for the analysis of milks commercially available. Results: ICP-AES for determination of Cd, Cr, Cu, Mn, and Ni was linear over a certain concentration range with a coefficient correlation value of>0.997. The limit of quantification values of Cd, Cr, Cu, Mn, and Ni were 0.0047; 0.0050; 0.0066; 0.0061; and 0.0169 µg/ml, respectively. The precision of analytical method exhibited relative standard deviation (RSD) values of 3.18%; 4.17%; 3.05%; 2.93%; and 4.47% during repeatability test and 5.28%; 5.06%; 3.67%; 3.67%; and 11.17% during intermediate precision of Cd, Cr, Cu, Mn, and Ni respectively. The recoveries of these metals assessed using standard addition method were 92.25; 90.88; 102.87; 94.50; and 86.85%, respectively. Conclusion: ICP-AES offered a reliable and fast method for the determination of heavy metals in milk products. The developed method could be proposed as an official method for determination of heavy metals in milk products.

scholarly journals Development and Validation of an Analytical Method for Carnosol, Carnosic Acid and Rosmarinic Acid in Food Matrices and Evaluation of the Antioxidant Activity of Rosemary Extract as a Food Additive

Antioxidants ◽  
2019 ◽  
Vol 8 (3) ◽  
pp. 76 ◽  
Author(s):  
Seung-Hyun Choi ◽  
Gill-Woong Jang ◽  
Sun-Il Choi ◽  
Tae-Dong Jung ◽  
Bong-Yeon Cho ◽  
...  
Keyword(s):  
Antioxidant Activity ◽  
Analytical Method ◽  
High Performance ◽  
Limit Of Detection ◽  
Acid Value ◽  
Food Additive ◽  
Carnosic Acid ◽  
Rosemary Extract ◽  
Relative Standard ◽  
Food Matrices

Antioxidants are used to prevent the oxidation of foods. When used for food additive purposes, the dosage should be regulated and the functionality evaluated to ensure stability. In this study, we performed a method validation for the quantitative analysis of rosemary extract residues and evaluated the antioxidant activity of rosemary extract in food matrices. The validated method was able to determine rosemary extract under the optimized high-performance liquid chromatography-photodiode array (HPLC-PDA) conditions. Furthermore, the antioxidant activity was evaluated by peroxide value, acid value, and in terms of the residual antioxidant levels in lard oil. For HPLC-PDA analysis, the limit of detection and quantification of rosemary extracts was ranged from 0.22 to 1.73 μg/mL, 0.66 to 5.23 μg/mL and the recoveries of the rosemary extracts ranged from 70.6 to 114.0%, with relative standard deviations of between 0.2% and 3.8%. In terms of antioxidant activity, carnosic acid performed better than carnosol. Furthermore, by evaluation of the residual antioxidant level using HPLC, we found that carnosic acid is more stable in lard oil than carnosol. These results indicate that rosemary extract can be used as an antioxidant and that the analytical method is suitable for the determination of rosemary extract in various food samples.

scholarly journals METHOD DEVELOPMENT AND VALIDATION FOR ANALYSIS OF DEOXYARBUTININ ANHYDROUS EMULSION SYSTEM USING HIGH-PERFORMANCE LIQUID CHROMATOGRAPHY

2019 ◽  
pp. 172-175 ◽  
Author(s):  
MUCHTARIDI MUCHTARIDI ◽  
IDA MUSFIROH ◽  
AHMAD FAUZI
Keyword(s):  
High Performance Liquid Chromatography ◽  
Liquid Chromatography ◽  
Analytical Method ◽  
High Performance ◽  
Method Development ◽  
Limit Of Detection ◽  
Internal Standard ◽  
Emulsion System ◽  
Relative Standard ◽  
Limit Of Quantitation

Objective: The aim of this study is to develop a simple, precise and accurate analytical method of deoxyarbutin in anhydrous emulsion system preparation. Methods: The analysis was conducted using high-performance liquid chromatography (HPLC). Chromatographic analysis was carried out using a reversed phase-C18 column. The mobile consists of two phases methanol and water (60: 40 v/v) at a flow rate of 1.0 ml/min. The determinations were performed using UV detector set at 225 nm. All validation procedures were added with hydroquinone as an internal standard. Results: The method showed coefficient correlation is 0.9978, relative standard deviation (RSD) smaller than 2%, Limit of Detection (LOD) and Limit of Quantitation (LOQ) are 0.599 µg/ml and 1.817 µg/ml respectively. The total amount deoxyarbutin in anhydrous emulsion preparation is 1.964+0.02 % with 98% recovery percentage. Conclusion: The developed HPLC analytical method meets the validation criteria made by International Conference on Harmonisation (ICH).

scholarly journals Ultrasensitive bioassaying of HER-2 protein for diagnosis of breast cancer using reduced graphene oxide/chitosan as nanobiocompatible platform

2021 ◽  
Vol 12 (1) ◽  
Author(s):  
Hassan Nasrollahpour ◽  
Ibrahim Isildak ◽  
Mohammad-Reza Rashidi ◽  
Esmat Alsadat Hashemi ◽  
Abdolhosein Naseri ◽  
...  
Keyword(s):  
Breast Cancer ◽  
Graphene Oxide ◽  
Reduced Graphene Oxide ◽  
Limit Of Detection ◽  
Test Method ◽  
Reduced Graphene ◽  
Relative Standard ◽  
Carboxylic Groups ◽  
Her 2 ◽  
Amine Groups

Abstract Background In this label-free bioassay, an electrochemiluminescence (ECL) immunosensor was developed for the quantification of breast cancer using HER-2 protein as a metastatic biomarker. Method For this purpose, the ECL emitter, [Ru(bpy)3]2+, was embedded into biocompatible chitosan (CS) polymer. The prepared bio-composite offered high ECL reading due to the depletion of human epidermal growth factor receptor 2 (HER-2) protein. Reduced graphene oxide (rGO) was used as substrate to increase signal stability and achieve greater sensitivity. For this, rGO was initially placed electrochemically on the glassy carbon electrode (GCE) surface by cyclic voltammetry (CV) technique. Next, the prepared CS/[Ru(bpy)3]2+ biopolymer solution was coated on a drop of the modified electrode such that the amine groups of CS and the carboxylic groups of rGO could covalently interact. Using EDC/NHS chemistry, monoclonal antibodies (Abs) of HER-2 were linked to CS/[Ru(bpy)3]2+/rGO/GCE via amide bonds between the carboxylic groups of Ab molecules and amine groups of CS. The electrochemical behavior of the electrode was studied using different electrochemical techniques such as electrochemical impedance spectroscopy (EIS), differential pulse voltammetry (DPV) and square wave voltammetry (SWV) and also ECL tests. Results After passing all optimization steps, the lower limit of detection (LLOQ) and linear dynamic range (LDR) of HER-2 protein were practically obtained as 1 fM and 1 fM to 1 nM, individually. Importantly, the within and between laboratory precisions were performed and the suitable relative standard deviations (RSDs) were recorded as 3.1 and 3.5%, respectively. Conclusions As a proof of concept, the designed immunosensor was desirably applied for the quantification of HER-2 protein in breast cancer suffering patients. As a result, the designed ECL-based immunosensor has the capability of being used as a conventional test method in biomedical laboratories for early detection of HER-2 protein in biological fluids. Graphic Abstract

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