Certification of Ochratoxin A Reference Materials: Calibration Solutions OTAN-1 and OTAL-1 and a Mycotoxin-Contaminated Rye Flour MYCO-1

2019 ◽  
Vol 102 (6) ◽  
pp. 1756-1766 ◽  
Author(s):  
Jennifer Bates ◽  
Adilah Bahadoor ◽  
Yi Cui ◽  
Juris Meija ◽  
Anthony Windust ◽  
...  
Keyword(s):  
Ochratoxin A ◽  
Mass Fraction ◽  
Method Development ◽  
Primary Standard ◽  
Internal Standard ◽  
Rye Flour ◽  
Regulatory Testing ◽  
Calibration Solution ◽  
Double Isotope ◽  
Global Food

Background: Among the regulated mycotoxins that contaminate global food supplies, ochratoxin A is particularly harmful as a nephrotoxin and suspected carcinogen. Objective: To support global measurement comparability, certified calibration solutions for ochratoxin A and [13C6]-ochratoxin A (OTAN-1 and OTAL-1, respectively) as well as a mycotoxin-contaminated rye flour certified reference material (CRM) known as MYCO-1 were developed. Methods: Quantitative proton NMR was used along with maleic acid as an external standard traceable to the Système international (SI) to measure the concentration of ochratoxin A and [13C6]-ochratoxin A for the calibration solutions. OTAN-1 and OTAL-1 were then used as a pair in double isotope dilution MS to certify the mass fraction of ochratoxin A in MYCO-1. The natural ochratoxin A CRM served as the primary standard for traceable quantitation, while the synthetic [13C6]-ochratoxin A CRM served as the internal standard. Results: The certified mass fraction of ochratoxin A or [13C6]-ochratoxin A in the two mycotoxin calibration solution standards was established to be 11.03 ± 0.32 µg/g (k = 2) for OTAN-1 and 4.89 ± 0.18 µg/g (k = 2) for OTAL-1. The mass fraction of ochratoxin A in the rye flour standard MYCO-1 was certified at 4.05 ± 0.88 µg/kg (k = 2). Conclusions: These CRMs will support regulatory testing as they can be used in the method development, validation, calibration, and QC analysis of ochratoxin A. Highlights: This report highlights the methods used to certify OTAN-1, OTAL-1, and MYCO-1 as well as the challenges associated with producing such materials, which can be applied to a wide variety of other CRMs.

Certification of Ochratoxin A Reference Materials: Calibration Solutions OTAN-1 and OTAL-1 and a Mycotoxin-Contaminated Rye Flour MYCO-1

2019 ◽  
Vol 102 (6) ◽  
pp. 1756-1766
Author(s):  
Jennifer Bates ◽  
Adilah Bahadoor ◽  
Yi Cui ◽  
Juris Meija ◽  
Anthony Windust ◽  
...  
Keyword(s):  
Ochratoxin A ◽  
Mass Fraction ◽  
Method Development ◽  
Primary Standard ◽  
Internal Standard ◽  
Rye Flour ◽  
Regulatory Testing ◽  
Calibration Solution ◽  
Double Isotope ◽  
Global Food

Abstract Background: Among the regulated mycotoxins that contaminate global food supplies, ochratoxin A is particularly harmful as a nephrotoxin and suspected carcinogen. Objective: To support global measurement comparability, certified calibration solutions for ochratoxin A and [13C6]-ochratoxin A (OTAN-1 and OTAL-1, respectively) as well as a mycotoxin-contaminated rye flour certified reference material (CRM) known as MYCO-1 were developed. Methods: Quantitative proton NMR was used along with maleic acid as an external standard traceable to the Système international (SI) to measure the concentration of ochratoxin A and [13C6]-ochratoxin A for the calibration solutions. OTAN-1 and OTAL-1 were then used as a pair in double isotope dilution MS to certify the mass fraction of ochratoxin A in MYCO-1. The natural ochratoxin A CRM served as the primary standard for traceable quantitation, while the synthetic [13C6]-ochratoxin A CRM served as the internal standard. Results: The certified mass fraction of ochratoxin A or [13C6]-ochratoxin A in the two mycotoxin calibration solution standards was established to be 11.03 ± 0.32 µg/g (k = 2) for OTAN-1 and 4.89 ± 0.18 µg/g (k = 2) for OTAL-1. The mass fraction of ochratoxin A in the rye flour standard MYCO-1 was certified at 4.05 ± 0.88 µg/kg (k = 2). Conclusions: These CRMs will support regulatory testing as they can be used in the method development, validation, calibration, and QC analysis of ochratoxin A. Highlights: This report highlights the methods used to certify OTAN-1, OTAL-1, and MYCO-1 as well as the challenges associated with producing such materials, which can be applied to a wide variety of other CRMs.

Bioanalytical Method Development and Validation for the Determination of Vasopressin Receptor Antagonist Conivaptan in Mouse Plasma at NanoLevel and its Pharmacokinetic Application

2019 ◽  
Vol 15 (5) ◽  
pp. 591-598 ◽  
Author(s):  
Haitham Alrabiah ◽  
Ahmed Bakheit ◽  
Sabray Attia ◽  
Gamal A.E. Mostafa
Keyword(s):  
Method Development ◽  
Internal Standard ◽  
Vasopressin Receptor ◽  
Mouse Plasma ◽  
Precipitation Procedure ◽  
Validation Parameters ◽  
The Us ◽  
Method Development And Validation ◽  
Development And Validation

Background: Conivaptan inhibits two of vasopressin receptor (vasopressin receptor V1a and V2). Conivaptan is used for the treatment of hyponatremia, and in some instances, for the treatment of the heart failure. Methods: The present study aimed to develop a simple, sensitive, and accurate HPLC with ultraviolet detection for the assay of conivaptan (CON) in mouse plasma using bisoprolol as internal standard (IS). A precipitation procedure was used to extract CON and the IS from the mouse plasma. CON was chromatographically separated using a C18 analytical column at 25°C. The separation was carried out using a mixture of phosphate buffer (50 mM): acetonitrile (60: 40, v/v, pH 4.5) with a flow rate of 1.0 mL/min and detection was performed at 240 nm. Results: The assay was validated according to the US Food and Drug (FDA) guidelines. The method demonstrated linearity over a concentration range of 150 - 2000 ng/mL (correlation coefficient: r 2 = 0.9985). The mean recovery of CON from the mouse plasma was 101.13%. All validation parameters for CON were within the acceptable range. Conclusion: The investigated method has been shown to be suitable for estimating the CON in plasma samples, and this method is sensitive and highly selective, allowing the estimation of its concentrations up to the nano-scale. The suggested method was successfully used in a pharmacokinetic study of CON in mouse plasma.

Bioanalytical method development and validation of simultaneous analysis of telmisartan and hydrochlorthiazide in human plasma using LC-MS/MS

2016 ◽  
Vol 5 (03) ◽  
pp. 4862 ◽  
Author(s):  
Mathew George* ◽  
Lincy Joseph ◽  
Arpit Kumar Jain ◽  
Anju V.
Keyword(s):  
Human Plasma ◽  
Retention Time ◽  
High Performance ◽  
Method Development ◽  
Matrix Effects ◽  
Solid Phase ◽  
Internal Standard ◽  
Assay Method ◽  
Buffer System ◽  
Internal Standards

A simple, sensitive, rapid and economic high performance thin layer chromatographic method and a mass spectroscopic assay method has been developed for the quantification of telmisartan and hydrochlorthiazide combination in human plasma. The internal standards and analytes were extracted from human plasma by solid-phase extraction with HLB Oasis1cc (30mg) catridges. The scanning and optimization for the samples are done using methanol: water (50:50). The samples were chromatographed using reverse phase chromatography with C-18 column of different manufacturers like Ascentis C18 (150×4. 6, 5µ) using the buffer system Acetonitrile: Buffer (80:20%v/v) which consist of 2±0. 1Mm ammonium format at a flow rate of 0. 7ml/min at a column oven temperature 35±10c. The internal standard used was hydrochlorthiazide13c1, d2 and telmisartand3. The extraction techniques include conditioning, loading, washing and elution, drying followed by reconstitution of the dried samples. The volume injected was 10µl with the retention time of 3-4 min for telmisartan, 1-2 min for hydrochlorthiazide and for the internal standards the retention time was 3-4 min for telmisartand3 and 1-2 min for hydrochlorthiazide c13d2. The rinsing solution was Acetonitrile: HPLC grade water in the ratio (50:50). The above developed method was validated using various parameters like selectivity and sensitivity, accuracy and precision, matrix effects, % recovery and various stability studies. The method was proved to be sensitive, accurate, precise and reproducible. The preparation showed high recovery for the quantitative determination of telmisartan and hydrochlorthiazide in human plasma.

scholarly journals Occurrence of mycotoxins in selected agricultural and commercial products available in eastern Poland

2021 ◽  
Vol 19 (1) ◽  
pp. 653-664
Author(s):  
Grażyna Kowalska ◽  
Radosław Kowalski
Keyword(s):  
Ochratoxin A ◽  
Aflatoxin B1 ◽  
Extraction Method ◽  
Maximum Allowable Concentration ◽  
Commercial Products ◽  
Ms Analysis ◽  
Rye Flour ◽  
Three Samples ◽  
Aflatoxin B2

Abstract The objective of this study was the estimation of the content of 13 mycotoxins (diacetoxyscirpenol, T-2 toxin, HT-2 toxin, nivalenol, deoxynivalenol, 3-acetyldeoxynivalenol, fusarenone X, aflatoxin B1, aflatoxin B2, aflatoxin G1, aflatoxin G2, ochratoxin A, and zearalenone) in various products from the eastern part of Poland. The content of mycotoxins in the analysed samples was assayed using the extraction method combined with HPLC-MS/MS analysis. We found mycotoxins in 25 of the 92 samples tested (27%). Contamination with mycotoxins was noted most frequently in samples of cereals – 56% – and also in samples of flour and cocoa, in which a content of mycotoxins was noted in 24 and 16% of the samples, respectively. The most frequently identified were the following – deoxynivalenol detected in 18 samples (72%), zearalenone detected in eight samples (32%), toxin HT-2 detected in four samples (16%), ochratoxin A identified in three samples (12%), and toxin T-2 detected in one sample (4%). In one analysed sample of mixed flour and in one analysed sample of wheat and rye flour, the maximum allowable concentration was exceeded in the case of two identified mycotoxins – deoxynivalenol (2,250 μg/kg) and ochratoxin A (15.6 and 17.1 μg/kg).

scholarly journals Comparison of Flow Injection-MS/MS and LC-MS/MS for the Determination of Ochratoxin A

Toxins ◽  
2021 ◽  
Vol 13 (8) ◽  
pp. 547
Author(s):  
Kai Zhang
Keyword(s):  
Ochratoxin A ◽  
Flow Injection ◽  
Internal Standard ◽  
Grape Juice ◽  
Tandem Mass ◽  
Triple Quadrupole ◽  
On Line ◽  
Red Grape Juice ◽  
Red Grape

Two methods for measuring ochratoxin A in corn, oat, and grape juice were developed and compared. Flow injection (FI) and on-line liquid chromatography (LC) performances were evaluated separately, with both methods using a triple quadrupole tandem mass spectrometer (MS/MS) for quantitation. Samples were fortified with 13C uniformly labeled ochratoxin A as the internal standard (13C-IS) and prepared by dilution and filtration, followed by FI- and LC-MS/MS analysis. For the LC-MS/MS method, which had a 10 min run time/sample, recoveries of ochratoxin A fortified at 1, 5, 20, and 100 ppb in corn, oat, red grape juice, and white grape juice ranged from 100% to 117% with RSDs < 9%. The analysis time of the FI-MS/MS method was <60 s/sample, however, the method could not detect ochratoxin A at the lowest fortification concentration, 1 ppb, in all tested matrix sources. At 5, 20, and 100 ppb, recoveries by FI-MS/MS ranged from 79 to 117% with RSDs < 15%. The FI-MS/MS method also had ~5× higher solvent and matrix-dependent instrument detection limits (0.12–0.35 ppb) compared to the LC-MS/MS method (0.02–0.06 ppb). In the analysis of incurred corn and oat samples, both methods generated comparable results within ±20% of reference values, however, the FI-MS/MS method failed to determine ochratoxin A in two incurred wheat flour samples due to co-eluted interferences due to the lack of chromatographic separation.

Influence of flour from oilseed meal on sugars content in rye bread

2021 ◽  
Vol 9 (16) ◽  
pp. 57-68
Author(s):  
Halyna Voloshchuk ◽  
Keyword(s):  
Chemical Composition ◽  
Mass Fraction ◽  
Raw Materials ◽  
Sugar Content ◽  
Jerusalem Artichoke ◽  
Oilseed Meal ◽  
Rye Bread ◽  
Rye Flour ◽  
Pumpkin Seeds ◽  
The Impact

Subject of research – sugar content in rye bread with fractionally defatted flour from walnuts, pumpkin seeds, sesame and Jerusalem artichoke powder. The purpose – to investigate the chemical composition of sugars in flour from oilseed meal and to explain the impact of new raw materials upon the sugar content in bread made from rye flour. Materials and methods. For the production of pilot of bread used: rye flour; fermented rye malt; table salt; drinking water; ready liquid rye sourdough (composition: Lactobacillus plantarum 30, L .casei 26, L. fermenti 34, L .brevis and Saccharomyces minor "Chernorichenskaya", S. cerevisiae L1); fractionally defatted flour from walnuts, pumpkin seeds and sesame produced by PE "Research and Production Company "Elitfito"; Jerusalem artichoke powder "Dar". The dough was prepared in a three-phase way: liquid sourdough – saccharified choux – dough. Jerusalem artichoke powder and oilseed meal were added to the dough. The chemical composition of sugars in raw materials and bread was determined by high-performance liquid chromatography. The effect of fractionally defatted flour on the course of processes in rye dough was performed on a farinograph and amylograph of Brabender. The intensity of gas formation of the dough was determined on the device AG-1. Changes in the crystal structure of the bread crumb were performed using X-ray phase analysis on the device DRON UM-1 in the range of angles 2θ from 5 to 60 degrees. Results. It is established that the share of sugars in flour from oilseed meal is 2 ... 8 times higher than the content of sugars in rye flour. The content of sugars in fractionally defatted flour from walnuts is 43.0 %, from pumpkin seeds – 14.2 %, from sesame – 12.8% by weight of dry matter. Up to 80% of all sugars in fractionally defatted flour are sucrose and maltose. The ratio of fructose to glucose in fractionally defatted flour from walnuts is 1:1.25; from pumpkin seeds – 1:0.73; of sesame seeds – 1:0.5. The addition of 7.0 % fractionally defatted flour mixed with 3 % of the Jerusalem artichoke powder reduces the mass fraction of sugars in bread compared to the bread made with Jerusalem artichoke only. It has been studied that fractionally defatted flour from walnuts, pumpkin seeds and sesame reduces the hydrolytic decomposition of rye flour starch and promotes the process of fermentation of sugars. Scope. A mixture of fractionally defatted flour from oilseed meal in the amount of 7 % should be used for the production of bread from rye flour with 3 % Jerusalem artichoke powder to the mass fraction of flour to reduce the content of high glycemic starch sugars.

scholarly journals NEW METHOD DEVELOPMENT AND VALIDATION FOR THE DETERMINATION OF FEBUXOSTAT IN HUMAN PLASMA BY LIQUID CHROMATOGRAPHY–MASS SPECTROMETRY

2016 ◽  
Vol 8 (9) ◽  
pp. 61 ◽  
Author(s):  
Narottam Pal ◽  
Avanapu Srinivasa Rao ◽  
Pigilli Ravikumar
Keyword(s):  
Mass Spectrometry ◽  
Liquid Chromatography ◽  
Human Plasma ◽  
Method Development ◽  
Multiple Reaction Monitoring ◽  
Internal Standard ◽  
New Method ◽  
Liquid Chromatography Mass Spectrometry ◽  
Chromatography Mass Spectrometry

<p><strong>Objective</strong>:<strong> </strong>To develop a new method and validate the same for the determination of Febuxostat (FBS) in human plasma by liquid chromatography–mass spectrometry (LCMS).</p><p><strong>Methods</strong>:<strong> </strong>The present method utilized reversed-phase high-performance liquid chromatography with tandem mass spectroscopy. Febuxostat D9 (FBS D9) was used as internal standard (IS). The analyte and internal standard were separated from human plasma by using solid phase extraction method. Zorbax Eclipse XDB, C<sub>8</sub>, 100 mm x 4.6 mm, 3.5 µm column was used and HPLC grade acetonitrile, 5 millimolar (mM) ammonium format (80: 20, v/v) as mobile phase, detected by mass spectrometry operating in positive ion and multiple reaction monitoring modes.</p><p><strong>Results</strong>:<strong> </strong>The parent and production transitions for FBS and internal standard were at m/z 317.1→261.0 and 326.1→262.0 respectively. The method was validated for system suitability, specificity, carryover effect, linearity, precision, accuracy, matrix effect, sensitivity and stability. The linearity range was from 20.131 ng/ml to10015. 534 ng/ml with a correlation coefficient of 0.999. Precision results (%CV) across six quality control samples were within the limit. The percentage recovery of FBS and internal standard from matrix samples was found to be 76.57% and 75.03% respectively.</p><p><strong>Conclusion</strong>:<strong> </strong>Present study describes new LC-MS method for the quantification of FBS in a pharmaceutical formulation. According to validation results, it was found to be a simple, sensitive, accurate and precise method and also free from any kind of interference. Therefore the proposed analytical method can be used for routine analysis for the estimation of FBS in its formulation.</p>

Detection of ochratoxin A based on the use of its diastereoisomer as an internal standard

2014 ◽  
Vol 6 (15) ◽  
pp. 5610-5614 ◽  
Author(s):  
Mohamed Attya ◽  
Leonardo Di Donna ◽  
Fabio Mazzotti ◽  
Alessia Fazio ◽  
Bartolo Gabriele ◽  
...  
Keyword(s):  
Ochratoxin A ◽  
Internal Standard ◽  
Standard Approach

A new methodology for the determination of ochratoxin A (OTA) was developed using a diastereoisomeric internal standard approach and HPLC-FLD.

scholarly journals RP-HPLC method development and validation for estimation of rivaroxaban in pharmaceutical dosage forms

2013 ◽  
Vol 49 (2) ◽  
pp. 359-366 ◽  
Author(s):  
Mustafa Çelebier ◽  
Tuba Reçber ◽  
Engin Koçak ◽  
Sacide Altinöz
Keyword(s):  
Method Development ◽  
Internal Standard ◽  
Hplc Method ◽  
Pharmaceutical Dosage Forms ◽  
Rp Hplc ◽  
Ich Guidelines ◽  
Method Development And Validation ◽  
Hplc Method Development ◽  
Development And Validation ◽  
Tablet Dosage

Rivaroxaban, an anti-clotting medication, acts at a crucial point in the blood-clotting process and stops the formation of blood clots. In this study, RP-HPLC method was developed for the determination of rivaroxaban in tablets (Xarelto® (10 mg)). Phenomenex Luna 5 µm C18 100 Å LC Column (250 x 4.6 mm) was used at 40 ºC. Isocratic elution was performed with ACN:Water (55:45 v/v) mixture. The flow rate was 1.2 mL min-1 and UV detection was at 249 nm. Internal standard (Caffeine) and rivaroxaban were eluted within 2.21 and 3.37 minutes, respectively. The developed method was validated according to the ICH guidelines and found to be linear within the range 0.005 - 40.0 µg mL-1. The method was accurate, precise, robust and rapid. Thus, it was applied successfully for the quality control assay of rivaroxaban in tablet dosage form.

scholarly journals Bioanalytical Method Development and Validation for Determination of Sulfasalazine in Rabbit Plasma by HPLC-UV

2021 ◽  
Vol 33 (7) ◽  
pp. 1692-1698
Author(s):  
S.S. Jadiya ◽  
N. Upmanyu ◽  
S. Arulmozhi ◽  
V. Jain ◽  
S. Sankaran ◽  
...  
Keyword(s):  
High Performance ◽  
Method Development ◽  
High Efficiency ◽  
Internal Standard ◽  
Ultra Violet ◽  
Precipitation Method ◽  
Pharmacokinetic Studies ◽  
Rabbit Plasma ◽  
Bioanalytical Method

In present study, an advanced, simple and a rapid reverse phase high performance liquid chromatography (RP-HPLC) method was developed for the quantitative determination of sulfasalazine in rabbit plasma. Sulfasalazine was separated using Chromatopak C-18 basic peerless (250 mm × 4.6 mm, 5μ) column in an isocratic mode using mobile phase consisting of the mixture of 10mM Ammonium acetate pH adjusted to 4.5 and acetonitrile (70:30 v/v) with a flow rate of about 1.0 mL/min at ambient temperature. An ultra-violet detection of sulfasalazine and the internal standard was carried out at 362 nm. Both sulfasalazine and internal standard (IS, 4-hydroxy benzoate) were extracted from plasma matrices with high efficiency using a simple protein precipitation method. The method was found to be highly selective with no carryover effects. Linearity of sulfasalazine was found with the range of 2.5-100 μg/mL with the value of r2 > 0.995 a correlation coefficient. At all three quality control levels, developed bioanalytical method was found as repeatable and reproducible as well. The average recoveries of sulfasalazine from plasma were in the range of 95.59-97.16%. The bioanalytical samples showed good and acceptable stability of sulfasalazine solution at different storage, packaging and handling conditions. Hence, in conclusion, the validated and developed HPLC-UV method could be effectively utilized for determination of sulfasalazine in pharmacokinetic studies involving novel formulations.

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