Determination of T-2/HT-2 toxins in duplicate diets in the Netherlands by GC-MS/MS: method development and estimation of human exposure

2014 ◽  
Vol 7 (3) ◽  
pp. 267-276 ◽  
Author(s):  
A.A. Jekel ◽  
H.P. van Egmond
Keyword(s):  
Body Weight ◽  
The Netherlands ◽  
Method Development ◽  
Daily Intake ◽  
Dietary Exposure ◽  
Limit Of Quantification ◽  
Pooled Samples ◽  
Duplicate Diets ◽  
Current Exposure

T-2 and HT-2 toxins (T-2 and HT-2) are important trichothecenes. They have been subject of formal risk assessment by various organisations, including the European Food Safety Authority (EFSA). The EFSA CONTAM Panel recently established a group Tolerable Daily Intake (TDI) of 100 ng/kg body weight/day for the sum of T-2 and HT-2. To assess the actual dietary exposure of Dutch consumers to T-2 and HT-2 a study was conducted in the Netherlands, in which duplicate portions of 24-h diets collected in 2011 were investigated for these toxins. This collection comprised 128 duplicate diets of the adult segment of the Dutch population, divided over a spring and autumn collection period. The diets in the study were homogenised and processed to lyophilised powders. Aliquots of every two of the samples were pooled to test portions that were analysed with a method, based on immunoaffinity chromatography clean-up in combination with GC-MS/MS determination. The method had a limit of quantification of 0.01 ?g/kg original non-lyophilised diet for both T-2 and HT-2. Recoveries ranged from 92-114% for T-2 and from 71-106% for HT-2, determined at levels of addition ranging from 0.1-0.3 ?g/kg. In practically all samples investigated, numerical values for the concentrations of T-2 and HT-2 could be obtained. Exposure estimates of the sum of T-2 and HT-2 in the 2011 study ranged from non-detectable to 18.6 ng/kg body weight/day. In addition limited sets of pooled samples of duplicate diets retained from collections in the period 1976-2004 were analysed for T-2 and HT-2. In all samples the mean and individual intakes of the sum of T-2 and HT-2 of the respondents were below the group TDI of the EFSA CONTAM Panel. From this study it was concluded that no health risks are expected from current exposure of adult Dutch consumers to T-2 and HT-2.

Determination of mean daily intakes of aflatoxin B1, aflatoxin M1, ochratoxin A, trichothecenes and fumonisins in 24-hour diets of children in the Netherlands

2009 ◽  
Vol 2 (4) ◽  
pp. 451-459 ◽  
Author(s):  
G. Bakker ◽  
E. Sizoo ◽  
A. Jekel ◽  
D.P. Pereboom-de Fauw ◽  
R. Schothorst ◽  
...  
Keyword(s):  
The Netherlands ◽  
Ochratoxin A ◽  
Daily Intake ◽  
Aflatoxin M1 ◽  
Limit Of Quantification ◽  
Diet Study ◽  
The Mean ◽  
Daily Intakes ◽  
Aflatoxin B

In 2006, a duplicate diet study of children's food was carried out in the Netherlands. Parents or guardians of 123 children collected duplicates of the 24-hour diets. Levels of aflatoxin M1, aflatoxin B1, ochratoxin A, trichothecenes and fumonisins were determined. Aflatoxin M1 was detectable in 10% of the samples, with all toxin levels below the limit of quantification. Aflatoxin B1 could be detected in 80% of the samples, while in 47% of all samples aflatoxin B1 was quantifiable. Ochratoxin A could be quantified in all samples. Deoxynivalenol was quantified in almost every sample, while T-2 and HT-2 toxins could only be quantified in 3.2% and 6.4% of the samples respectively. 15-acetyldeoxynivalenol was detected in 1.6% of the samples. Fumonisin B1 was detected in 28% of the samples and fumonisin B2 in a quarter of merely those samples where fumonisin B1 was detected. In 20% of the samples fumonisin B1 could be quantified and in a quarter of those samples fumonisin B2 could be quantified too. The analytical results were used to estimate levels of daily intake. Only the mean daily intake levels for aflatoxin B1, ochratoxin A, deoxynivalenol and fumonisins B1 and B2 could reliably be estimated. The values were 0.1, 4.1, 291 and 28 ng/kg bw/day respectively, all are well below the corresponding tolerable daily intakes. For aflatoxin B1 a tolerable intake does not exist, but the intake value for this mycotoxin was very low if compared to the value that would result from the intake of food, if it was contaminated with aflatoxin B1 at the EU regulatory limit, specified for baby food. The mean daily intakes of the mycotoxins determined in children's food in the Netherlands are low and implicate that there is no health risk for children due to exposure from the studied mycotoxins.

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 Determination of Fungi and Multi-Class Mycotoxins in Camelia sinensis and Herbal Teas and Dietary Exposure Assessment

Toxins ◽  
2020 ◽  
Vol 12 (9) ◽  
pp. 555
Author(s):  
Ingars Reinholds ◽  
Estefanija Bogdanova ◽  
Iveta Pugajeva ◽  
Laura Alksne ◽  
Darta Stalberga ◽  
...  
Keyword(s):  
Exposure Assessment ◽  
Daily Intake ◽  
Dietary Exposure ◽  
Fungal Species ◽  
Two Dimensional ◽  
Flight Mass Spectrometry ◽  
Low Concentrations ◽  
Exposure Levels ◽  
Tof Ms

In this paper, a study of fungal and multi-mycotoxin contamination in 140 Camellia sinensis and 26 herbal teas marketed in Latvia is discussed. The analysis was performed using two-dimensional liquid chromatography with time-of-flight mass spectrometry (2D-LC-TOF-MS) and MALDI-TOF-MS. In total, 87% of the tea samples tested positive for 32 fungal species belonging to 17 genera, with the total enumeration of moulds ranging between 1.00 × 101 and 9.00 × 104 CFU g−1. Moreover, 42% of the teas (n = 70) were contaminated by 1 to 16 mycotoxins, and 37% of these samples were positive for aflatoxins at concentrations ranging between 0.22 and 41.7 µg kg−1. Deoxynivalenol (DON) and its derivatives co-occurred in 63% of the tea samples, with their summary concentrations reaching 81.1 to 17,360 µg kg−1. Ochratoxin A (OTA), enniatins, and two Alternaria toxins were found in 10–37% of the teas at low concentrations. The dietary exposure assessment based on the assumption of a probable full transfer of determined mycotoxins into infusions indicated that the analysed teas are safe for consumers: the probable maximum daily exposure levels to OTA and the combined DON mycotoxins were only 0.88 to 2.05% and 2.50 to 78.9% of the tolerable daily intake levels.

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 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.

Risk assessment of chronic dietary exposure to the conjugated mycotoxin deoxynivalenol-3-β-glucoside in the Dutch population

2015 ◽  
Vol 8 (5) ◽  
pp. 561-572 ◽  
Author(s):  
E.M. Janssen ◽  
R.C. Sprong ◽  
P.W. Wester ◽  
M. De Boevre ◽  
M.J.B. Mengelers
Keyword(s):  
Risk Assessment ◽  
Body Weight ◽  
The Netherlands ◽  
Food Consumption ◽  
Upper Bound ◽  
Chronic Exposure ◽  
Dietary Exposure ◽  
Food Products ◽  
Dutch Population ◽  
Worst Case

In this study, a risk assessment of dietary exposure to the conjugated mycotoxin deoxynivalenol-3-β-glucoside (DON-3G) in the Dutch population was conducted. Data on DON-3G levels in food products available in the Netherlands are scarce. Therefore, data on co-occurring levels of DON-3G and deoxynivalenol (DON), its parent compound, were used to estimate the DON-3G/DON ratio for several food product categories. This resulted in a DON-3G/DON ratio of 0.2 (90% confidence interval (CI): 0.04-0.9) in grains & grain-milling products, 0.3 (90% CI: 0.03-2.8) in grain-based products and 0.8 (90% CI: 0.4-1.8) in beer. These ratios were applied to the Dutch monitoring data of DON to estimate the DON-3G concentrations in food products available in the Netherlands. DON and DON-3G concentrations were combined with food consumption data of two Dutch National Food Consumption Surveys to assess chronic exposure in young children (2-6 years), children (7-16 years) and adults (17-69 years) using the Monte Carlo Risk Assessment program. The chronic exposure levels of DON, DON-3G and the sum of both compounds (DON+DON-3G) were compared to the tolerable daily intake (TDI) of 1 μg/kg body weight/day which is based on the most critical effect of DON, namely decreased body weight gain. The assumption was made that DON-3G is deconjugated and then fully absorbed as DON in the gastro-intestinal tract. Exposure (P97.5) of the population aged 7-16 years and 17-69 years to DON or DON-3G separately, did not exceed the TDI. However, exposure to upper bound levels of DON+DON-3G (i.e. worst-case scenario) in the same age categories (P97.5) exceeded the TDI with a maximum factor of 1.3. Exposure (P97.5) of the 2-6 year-olds to DON was close to the TDI. Within this group, exposure (P97.5) to upper bound levels of DON+DON-3G exceeded the TDI with not more than a factor 2.

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

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 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.

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