scholarly journals Development of an LC-MS method for the semiquantitative determination of polyamide 6 contaminations in polyolefin recyclates

2020 ◽  
Author(s):  
Andrea Schweighuber ◽  
Markus Gall ◽  
Jörg Fischer ◽  
Yi Liu ◽  
Hermann Braun ◽  
...  
Keyword(s):  
Method Development ◽  
Negative Impact ◽  
Polyamide 6 ◽  
Limit Of Quantification ◽  
Assisted Extraction ◽  
Significant Negative Impact ◽  
Cyclic Oligomers ◽  
Marker Compounds ◽  
Cyclic Compounds

AbstractRecycling will be of increasing importance in the future, especially for plastic packaging waste mainly consisting of polyolefins. One major problem of recyclates comprises impurities which can have a significant negative impact on future product properties. Polyamide 6 can be found widely as contaminant in recycled polyolefins, leading to a need of quantification methods thereof. In this paper, a method development for the quantitative analysis of polyamide 6 is presented based on analysing ε-caprolactam and related cyclic oligomers as marker compounds in model recyclates of high- and low-density polyethylene and polypropylene compounded with low amounts of polyamide 6. For the method development and tentative identification of the different cyclic compounds, a HPLC-QTOF-MS was used and it was possible to detect six different compounds, ε-caprolactam and the corresponding cyclic di- to hexamer. The quantification was performed with a HPLC-QQQ-MS, equipped with a HILIC column, after sample preparation via microwave-assisted extraction. It could be shown that a good linearity from 0.2 up to 5 wt% polyamide 6 in the different polyolefins can be achieved. The cyclic trimer and tetramer show a low limit of quantification and are therefore well-suited for the quantification, whereas the other cyclic compounds can be then used as qualifiers to avoid false positives. To guarantee the applicability of the method, six real recyclate materials were analysed, whereby in three of them low amounts of polyamide 6 could be detected.

scholarly journals A novel LC-MS method development and validation for the determination of phenyl vinyl sulfone in eletriptan hydrobromide

2021 ◽  
Vol 7 (1) ◽  
Author(s):  
Indhu Priya Mabbu ◽  
G. Sumathi ◽  
N. Devanna
Keyword(s):  
Method Development ◽  
Limit Of Detection ◽  
Vinyl Sulfone ◽  
Limit Of Quantification ◽  
Relative Standard ◽  
Pressure Chemical Ionization ◽  
Pressure Chemical ◽  
Development And Validation ◽  
Phenyl Vinyl

Abstract Background The aim of the present method is to develop and validate a specific, sensitive, precise, and accurate liquid chromatography-mass spectrometry (LC-MS) method for the estimation of the phenyl vinyl sulfone in the eletriptan hydrobromide. The effective separation of the phenyl vinyl sulfone was achieved by the Symmetry C18 (50 × 4.6 mm, 3.5 μm) column and a mobile phase composition of 0.1%v/v ammonia buffer to methanol (5:95 v/v), using 0.45 ml/min flow rate and 20 μl of injection volume, with methanol used as diluent. The phenyl vinyl sulfone was monitored on atomic pressure chemical ionization mode mass spectrometer with positive polarity mode. Results The retention time of phenyl vinyl sulfone was found at 2.13 min. The limit of detection (LOD) and limit of quantification (LOQ) were observed at 1.43 ppm and 4.77 ppm concentration respectively; the linear range was found in the concentration ranges from 4.77 to 27.00 ppm with regression coefficient of 0.9990 and accuracy in the range of 97.50–102.10%. The percentage relative standard deviation (% RSD) for six replicates said to be injections were less than 10%. Conclusion The proposed method was validated successfully as per ICH guidelines. Hence, this is employed for the determination of phenyl vinyl sulfone in the eletriptan hydrobromide.

scholarly journals Total Fat Gravimetric Method Workflow in Portuguese Olives Using Closed-Vessel Microwave-Assisted Extraction (MAE)

Foods ◽  
2021 ◽  
Vol 10 (10) ◽  
pp. 2364
Author(s):  
João Gonçalo Lourenço ◽  
Daniel Ettlin ◽  
Inês Carrero Cardoso ◽  
Jesus M. Rodilla
Keyword(s):  
Limit Of Detection ◽  
Gravimetric Method ◽  
Reference Value ◽  
Microwave Assisted Extraction ◽  
Closed Vessel ◽  
Limit Of Quantification ◽  
Microwave Assisted ◽  
Assisted Extraction ◽  
Total Fat

A simple and rapid method for the quantitation of total fat in olive samples is designed, evaluated, and presented. This method is based on an innovative closed-vessel microwave-assisted extraction (MAE) technique. A method was designed for olives, and some figures of merits were evaluated: limit of detection (LOD), limit of quantification (LOQ) and expanded uncertainty (U). The data obtained in these experiences show that the workflow of the MAE method in a closed container is statistically equivalent to the other two methods, showing in this case better performance indicators (LOD = 0.02%, LOQ = 0.06%, and U = 15%). In addition, it is also demonstrated that the complete MAE method workflow allows the determination of total fat in a maximum of 12 analyses simultaneously for about 100 min in each run, which is the capacity of the rotor. This is a much better productivity when compared to the traditional Soxhlet-based method. Considering the sample workflow, the closed-vessel MAE method greatly simplifies sample handling, therefore minimizing sample loss during sample preparation and reducing analysis time. When MAE is compared to NIR-based methods, the advantage comes from there being no need for any type of calibration in the sample matrix. The MAE method itself can be used to determine the reference value for NIR calibration purposes. The results obtained for CRM using MAE were equivalent to the ones shown on the certificate.

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 Extraction and Determination of Vitamin K1 in Foods by Ultrasound-Assisted Extraction, SPE, and LC-MS/MS

Molecules ◽  
2020 ◽  
Vol 25 (4) ◽  
pp. 839 ◽  
Author(s):  
Yueqing Xu ◽  
Liangxiao Zhang ◽  
Ruinan Yang ◽  
Xu Yu ◽  
Li Yu ◽  
...  
Keyword(s):  
Formic Acid ◽  
Limit Of Detection ◽  
Solid Phase ◽  
Extraction Temperature ◽  
Vitamin K1 ◽  
Ultrasound Assisted Extraction ◽  
Limit Of Quantification ◽  
Assisted Extraction ◽  
Ultrasound Assisted

Vitamin K1 is one of the important hydrophobic vitamins in fat-containing foods. Traditionally, lipase is employed in the determination of vitamin K1 to remove the lipids, which makes the detection complex, time-consuming, and insensitive. In this study, the determination of vitamin K1 in fat-containing foods was developed based on ultrasound-assisted extraction (UAE), solid-phase extraction (SPE) combined with liquid chromatography–tandem mass spectrometry (LC-MS/MS). The optimal conditions for extraction of vitamin K1 were material–liquid ratio of 1:70 (g/mL), extraction temperature of 50 °C, extraction power of 700 W, extraction time of 50 min, material-wash fluid ratio of 1:60 (g/mL), and 8 mL of hexane/anhydrous ether (97:3, v/v) as the elution solvent. Then, vitamin K1 was analyzed on a ZORBAX SB-C18 column (50 mm × 2.1 mm, 1.8 μm) by gradient elution with water (0.01% formic acid) and methanol (0.01 formic acid + 2.5 mmol/L ammonium formate) as the mobile phase. The limit of detection (LOD) and limit of quantification (LOQ) were 0.05 and 0.16 μg/kg, respectively. Calibration curve was linear over the range of 10–500 ng/mL (R2 > 0.9988). The recoveries at three spiked levels were between 80.9% and 119.1%. The validation and application indicated that the proposed method was simple and sensitive in determination of vitamin K1 in fat-containing foods.

scholarly journals ULTRAVIOLET-SPECTROPHOTOMETRIC METHOD DEVELOPMENT AND VALIDATION FOR THE DETERMINATION OF NORFLOXACIN PRESENT IN TASTE MASKED DRUG RESIN COMPLEX

2018 ◽  
Vol 11 (4) ◽  
pp. 244
Author(s):  
Ayya Rajendra Prasad ◽  
Jayanthi Vijaya Ratna
Keyword(s):  
Spectrophotometric Method ◽  
Absorption Maximum ◽  
Method Development ◽  
Limit Of Detection ◽  
Statistical Parameters ◽  
Limit Of Quantification ◽  
Relative Standard ◽  
Validation Parameters ◽  
Development And Validation

 Objective: The objective of this study was developed and validated a novel, specific, precise, and simple ultraviolet (UV)-spectrophotometric method for the estimation of norfloxacin present in taste masked drug-resin complex.Methods: UV-spectrophotometric determination was performed with ELICO SL 1500 UV-visible spectrophotometer using 0.1 N HCl as a medium. The spectrum of the standard solution was run from 200 to 400 nm range for the determination of absorption maximum (λ max). λ max of norfloxacin was found at 278 nm. The absorbance of standard solutions of 1, 2, 3, 4, and 5 μg/ml of drug solution was measured at an absorption maximum at 278 nm against the blank. Then, a graph was plotted by taking concentration on X-axis and absorbance on Y-axis which gave a straight line. Validation parameters such as linearity and range, selectivity and specificity, limit of detection (LOD) and limit of quantification (LOQ), accuracy, precision, and robustness were evaluated as per the International Conference on Harmonization (ICH) guidelines.Results: Linearity for the UV-spectrophotometric method was noted over a concentration range of 1–5 μg/ml with a correlation coefficient of 0.9995. The LOD and LOQ for norfloxacin were found at 0.39 μg/ml and 1.19 μg/ml, respectively. Accuracy was in between 99.00% and 99.17%. % relative standard deviation for repeatability, intraday precision, and interday precision was found to be 0.600, in between 0.291 and 0.410, and in between 0.682 and 1.439, respectively. The proposed UV spectrophotometric method is found to be robust.Conclusion: The proposed UV-spectrophotometric method was validated according to the ICH guidelines, and results and statistical parameters demonstrated that the developed method is sensitive, precise, reliable, and simple for the estimation of norfloxacin present in taste masked drug-resin complex.

scholarly journals Method Development and Validation for Simultaneous Determination of Ezetimibe and Simvastatin In Combined Pharmaceutical Dosage Form By RP-HPLC Method

2013 ◽  
Vol 2 (2) ◽  
pp. 60-69 ◽  
Author(s):  
G Krishnaveni ◽  
PVV Sathyannarayana
Keyword(s):  
High Performance ◽  
Method Development ◽  
Limit Of Detection ◽  
High Performance Liquid Chromatographic ◽  
Simultaneous Estimation ◽  
Internal Diameter ◽  
Limit Of Quantification ◽  
Pharmaceutical Dosage Form ◽  
Pharmaceutical Dosage Forms

A simple, rapid reverse phase high-performance liquid chromatographic method was developed and validated for the simultaneous estimation of Ezetimibe and Simvastatin in bulk and pharmaceutical dosage forms. Chromatography was carried out by using Chromosil C-18,column having 250 x 4.6mm internal diameter with a mixture of Methanol:Acetonitrile:0.1%Orthophosphoric Aid in the ratio of 75:20:05 (v/v/v) as mobile phase. Determination of the different analytical parameters such as linearity, precision, accuracy, and specificity, limit of detection (LOD) and limit of quantification (LOQ) was done. The calibration curve was found to be linear for each analyte in the desired concentration range. The average recovery was found to be 99.88 and 100.12 for Ezetimibe and Simvastatin respectively. The proposed method is highly sensitive, precise and accurate, which was evident from the LOD value of 1.2ppm and 0.25ppm for Ezetimibe and Simvastatin respectively and hence the present method can be applied successfully for the quantification of active pharmaceutical ingredient (API) content in the combined formulations of Ezetimibe and Simvastatin. DOI: http://dx.doi.org/10.3329/ijpls.v2i2.15450 International Journal of Pharmaceutical and Life Sciences Vol.2(2) 2013: 60-69

Validation and application of an LC-MS/MS method for the determination of cyclic oligomers originating from polyamide 6 and polyamide 66 in food simulant

2018 ◽  
Vol 35 (7) ◽  
pp. 1410-1420 ◽  
Author(s):  
Oliver Kappenstein ◽  
Ingo Ebner ◽  
Carina Förster ◽  
Stephan Richter ◽  
Jürgen Weyer ◽  
...  
Keyword(s):  
Polyamide 6 ◽  
Polyamide 66 ◽  
Food Simulant ◽  
Cyclic Oligomers

scholarly journals The Arabic Version of MELASQoL Scale: Translation, Cultural Adaptation, with Assessment of Reliability and Validity

2021 ◽  
Vol 6 (2) ◽  
pp. 01-08
Author(s):  
Doaa AE Abou-Taleb ◽  
Alaa EA Moubasher ◽  
Ahmed K Ibrahim ◽  
Eman MK Youssef
Keyword(s):  
Cultural Adaptation ◽  
Negative Impact ◽  
High Reliability ◽  
Reliability And Validity ◽  
Severity Index ◽  
Arabic Version ◽  
Significant Negative Impact ◽  
The Impact

Background: Melasma has significant emotional and psychological effects and significant negative impact on patients’ quality of life (QoL). Melasma QoL Scale (MELASQoL) is a specific questionnaire that has been developed to assess the effect of melasma on patient’s QoL. Objective: Translation, cultural adaptation, reliability and validation of melasma specific QoL sale (MELASQoL) into Arabic. Patients and Methods: A total of 65 adult Egyptian female patients with melasma aged ≥18 years old with skin phototypes type III-V were enrolled in this study. Wood’s light was used for determination of the type of melasma either epidermal, dermal or mixed. Melasma severity was assessed by using the melasma area and severity index (MASI) score and the new modified score (mMASI). The impact of melasma on QoL was evaluated using the Arabic version of MELASQoL scale after translation and cultural adaptation according to the WHO guidelines. The questionnaire’s reliability and validity was assessed. Results: The internal consistency for the 10-item of the MELASQoL-A scale was excellent; Intra-class Correlation Coefficient (ICC) = 0.914 and Cronbach’s alpha coefficient (Cronbach α = 0.944) indicating high reliability of the developed Arabic version. There was significant positive correlation between the MELASQoL-A scale and the MASI score (r= 0.41; p= 0.0027), and the mMASI score (r = 0.36; p= 0.0032). Conclusion: The Arabic version of the MELASQoL scale was found to be a reliable and valid measure for evaluating the QoL among Egyptian melasma patients, supporting its use in Arab communities.

scholarly journals The RP-HPLC method development and validation for simultaneous determination of oryzalin and ethofumesate pesticides in soil and water

2021 ◽  
Author(s):  
Shishir Tandon ◽  
Suman Lata Pal
Keyword(s):  
Simultaneous Determination ◽  
Method Development ◽  
Hplc Method ◽  
Limit Of Quantification ◽  
Rp Hplc ◽  
Relative Standard ◽  
High Throughput Detection ◽  
Hplc Method Development ◽  
Soil And Water

Abstract A sensitive and reliable method for simultaneous determination of oryzalin and ethofumesate residues in pantnagar soil and water was validated. The compounds were extracted by LLE with dichloromethane from water, and acetone:methanol mixture from soil followed by SPE cleanup. Detection and quantification was done by RP-HPLC using mobile phase methanol:water (70:30, v/v) at 280 nm. The developed method showed satisfactory validation results with linearity (0.99), relative standard deviations (1.55 and 1.73%), and limit of quantification (0.002 μg g−1 and 0.005 μg g−1) for ethofumesate and oryzalin, respectively. Recoveries ranged for oryzalin and ethofumesate from 79.80–90.52, 75.58–86.04% (soil) and 83.50–95.92, 82.28–94.60% (water), respectively. The method could be used for routine high-throughput detection and determination of these compounds.

scholarly journals UV-SPECTROPHOTOMETRIC METHOD DEVELOPMENT AND VALIDATION FOR THE DETERMINATION OF LORNOXICAM IN MICROSPONGES

2018 ◽  
Vol 10 (1) ◽  
pp. 74 ◽  
Author(s):  
Ayya Rajendra Prasad ◽  
Bannaravuri Thireesha
Keyword(s):  
Spectrophotometric Method ◽  
Absorption Maximum ◽  
Method Development ◽  
Limit Of Detection ◽  
Statistical Parameters ◽  
Limit Of Quantification ◽  
Straight Line ◽  
Validation Parameters ◽  
Development And Validation

Objective: To develop and validate a novel, specific, precise and simple UV-spectrophotometric method for the estimation of lornoxicam present in microsponges.Methods: UV-spectrophotometric determination was performed with Thermo Scientific Evolution 201 UV-Vis spectrophotometer using methanol as a medium. The spectrum of the standard solution was run from 200-400 nm range for the determination of absorption maximum (λ max). λ max of lornoxicam was found at 353 nm. The absorbance of standard solutions of 3, 6, 9, 12 and 15, µg/ml of drug solution was measured at an absorption maximum at 353 nm against the blank. Then a graph was plotted by taking concentration on X-axis and absorbance on Y-axis which gave a straight line. Validation parameters such as linearity and range, selectivity and specificity, LOD and LOQ, accuracy, precision and robustness were evaluated as per ICH guidelines.Results: Linearity for the UV-spectrophotometric method was noted over a concentration range of 3.0-15.0 µg/ml with a correlation coefficient of 0.9995. The limit of detection (LOD) and limit of quantification (LOQ) for lornoxicam was found at 1.26 μg/ml and 3.82 μg/ml respectively. Accuracy was in between 99.21 and 99.60%. % RSD for repeatability, intraday precision and interday precision were found to be 0.473, in between 0.478 and 0.619 and in between 0.855 and 1.818 respectively. The proposed UV method is found to be robust.Conclusion: The proposed UV-Visible spectrophotometric method was validated according to the ICH guidelines and results and statistical parameters demonstrated that the developed method is sensitive, precise, reliable and simple for the estimation of lornoxicam present in microsponges.

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