Simultaneous quantification of vitamin E and vitamin E metabolites in equine plasma and serum using LC-MS/MS

2021 ◽  
pp. 104063872110054
Author(s):  
Hadi Habib ◽  
Carrie J. Finno ◽  
Ingrid Gennity ◽  
Gianna Favro ◽  
Erin Hales ◽  
...  
Keyword(s):  
Vitamin E ◽  
Normal Growth ◽  
Alpha Tocopherol ◽  
Limits Of Detection ◽  
Phase Gradient ◽  
Equine Plasma ◽  
Accuracy And Precision ◽  
Low Concentrations ◽  
Liquid Chromatography Tandem Mass ◽  
Acquity Uplc

Vitamin E deficiencies can impact normal growth and development in humans and animals, and assessment of circulating levels of vitamin E and its metabolites may be an important endpoint for evaluation. Development of a sensitive method to detect and quantify low concentrations of vitamin E and metabolites in biological specimens allows for a proper diagnosis for patients and animals that are deficient. We developed a method to simultaneously extract, detect, and quantify the vitamin E compounds alpha-tocopherol (α-TP), gamma-tocopherol (γ-TP), alpha-tocotrienol (α-TT), and gamma-tocotrienol (γ-TT), and the corresponding metabolites formed after β-oxidation of α-TP and γ-TP, alpha-carboxymethylbutyl hydroxychroman (α-CMBHC) and alpha- or gamma-carboxyethyl hydroxychroman (α- or γ-CEHC), respectively, from equine plasma and serum. Quantification was achieved through liquid chromatography–tandem mass spectrometry. We applied a 96-well high-throughput format using a Phenomenex Phree plate to analyze plasma and serum. Compounds were separated by using a Waters ACQUITY UPLC BEH C18 column with a reverse-phase gradient. The limits of detection for the metabolites and vitamin E compounds were 8–330 pg/mL. To validate the method, intra-day and inter-day accuracy and precision were evaluated along with limits of detection and quantification. The method was then applied to determine concentrations of these analytes in plasma and serum of horses. Alpha-TP levels were 3–6 µg/mL of matrix; the metabolites were found at much lower levels, 0.2–1.0 ng/mL of matrix.

scholarly journals Determination of Vitamin E in Cereal Products and Biscuits by GC-FID

2017 ◽  
Author(s):  
Ioannis N. Pasias ◽  
Ioannis K. Kiriakou ◽  
Lila Papakonstantinou ◽  
Charalampos Proestos
Keyword(s):  
Vitamin E ◽  
Low Cost ◽  
Alpha Tocopherol ◽  
Health Claims ◽  
Cereal Products ◽  
Accuracy And Precision ◽  
Good Accordance ◽  
First Time ◽  
Certified Values

A rapid, precise, accurate and low cost method for the determination of vitamin E (α-tocopherol) in cereal products and biscuits was developed. The uncertainty was calculated for the first time and the methods were performed in different cereal products and biscuits, characterized as “superfoods”. The limits of detection and quantification were calculated. Accuracy and precision were estimated using the certified reference material FAPAS T10112QC and the determined values were in good accordance with the certified values. The health claims according to the daily reference values for vitamin E were calculated and the results proved that the majority of the samples examined showed %daily value higher than 15%.

Alpha Tocopherol Loaded in Liposome: Preparation, Optimization, Characterization and Sperm Motility Protection

2020 ◽  
Vol 10 (3) ◽  
pp. 228-236 ◽  
Author(s):  
Lamia Taouzinet ◽  
Sofiane Fatmi ◽  
Allaeddine Khellouf ◽  
Mohamed Skiba ◽  
Mokrane Iguer-ouada
Keyword(s):  
Vitamin E ◽  
Sperm Motility ◽  
High Performance ◽  
Positive Impact ◽  
Alpha Tocopherol ◽  
Ethanol Injection ◽  
Liposome Preparation ◽  
Liposome Size ◽  
Optimum Solution ◽  
The Impact

Background: Alpha-tocopherol is a potent antioxidant involved in sperm protection particularly during cryopreservation. However, its poor solubility limits the optimal protection in aqueous solutions. Objective: The aim of this study was to enhance the solubility of α-tocopherol by the use of liposomes. Methods: The experimental approach consisted to load vitamin E in liposomes prepared by ethanol injection method and the optimization carried out by an experimental design. The optimum solution was characterized by high performance liquid chromatography and scanning electron microscope. Finely, the impact on sperm motility protection was studied by the freezing technic of bovine sperm. Results: The optimum solution was obtained when using 10.9 mg/ml of phospholipids, 1.7 mg/ml of cholesterol and 2 mg/ml of vitamin E. The liposome size was 99.86 nm, providing 78.47% of loaded efficiency. The results showed also a significant positive impact on sperm motility after hours of preservation. Conclusion: In conclusion, the current results showed the interest of liposome preparation as an alternative to enhance vitamin E solubility and to protect spermatozoa during cryopreservation.

scholarly journals Simplified and Rapid Determination of Primaquine and 5,6-Orthoquinone Primaquine by UHPLC-MS/MS: Its Application to a Pharmacokinetic Study

Molecules ◽  
2021 ◽  
Vol 26 (14) ◽  
pp. 4357
Author(s):  
Waritda Pookmanee ◽  
Siriwan Thongthip ◽  
Jeeranut Tankanitlert ◽  
Mathirut Mungthin ◽  
Chonlaphat Sukasem ◽  
...  
Keyword(s):  
Pharmacokinetic Study ◽  
High Performance ◽  
Rapid Determination ◽  
Active Metabolites ◽  
Chromatography Tandem Mass Spectrometry ◽  
Accuracy And Precision ◽  
The Matrix ◽  
Liquid Chromatography Tandem Mass ◽  
Isocratic Mode

The method for the determination of primaquine (PQ) and 5,6-orthoquinone primaquine (5,6-PQ), the representative marker for PQ active metabolites, via CYP2D6 in human plasma and urine has been validated. All samples were extracted using acetonitrile for protein precipitation and analyzed using the ultra-high-performance liquid chromatography–tandem mass spectrometry (UHPLC-MS/MS) system. Chromatography separation was carried out using a Hypersil GOLDTM aQ C18 column (100 × 2.1 mm, particle size 1.9 μm) with a C18 guard column (4 × 3 mm) flowed with an isocratic mode of methanol, water, and acetonitrile in an optimal ratio at 0.4 mL/min. The retention times of 5,6-PQ and PQ in plasma and urine were 0.8 and 1.6 min, respectively. The method was validated according to the guideline. The linearity of the analytes was in the range of 25–1500 ng/mL. The matrix effect of PQ and 5,6-PQ ranged from 100% to 116% and from 87% to 104% for plasma, and from 87% to 89% and from 86% to 87% for urine, respectively. The recovery of PQ and 5,6-PQ ranged from 78% to 95% and form 80% to 98% for plasma, and from 102% to from 112% to 97% to 109% for urine, respectively. The accuracy and precision of PQ and 5,6-PQ in plasma and urine were within the acceptance criteria. The samples should be kept in the freezer (−80 °C) and analyzed within 7 days due to the metabolite stability. This validated UHPLC-MS/MS method was beneficial for a pharmacokinetic study in subjects receiving PQ.

scholarly journals Development and Validation of a Sensitive, Specific and Reproducible UPLC-MS/MS Method for the Quantification of OJT007, A Novel Anti-Leishmanial Agent: Application to a Pharmacokinetic Study

2021 ◽  
Vol 18 (9) ◽  
pp. 4624
Author(s):  
Maria Rincon Nigro ◽  
Jing Ma ◽  
Ololade Tosin Awosemo ◽  
Huan Xie ◽  
Omonike Arike Olaleye ◽  
...  
Keyword(s):  
Formic Acid ◽  
High Performance ◽  
Leishmania Major ◽  
Internal Standard ◽  
Gradient Elution ◽  
Rat Plasma ◽  
The Matrix ◽  
Liquid Chromatography Tandem Mass ◽  
Positive Mode ◽  
Acquity Uplc

OJT007 is a methionine aminopeptidase 1 (MetAP1) inhibitor with potent anti-proliferative effects against Leishmania Major. In order to study its pharmacokinetics as a part of the drug development process, a sensitive, specific, and reproducible ultra-high performance liquid chromatography-tandem mass spectrometry (UPLC-MS/MS) method was developed and validated. Voriconazole was used as the internal standard to generate standard curves ranging from 5 to 1000 ng/mL. The separation was achieved using a UPLC system equipped with an Acquity UPLC BEH C18 column (2.1 × 50 mm, 1.7 μm) with 0.1% formic acid in acetonitrile and 0.1% formic acid in water as the mobile phase under gradient elution at a flow rate of 0.4 mL/min. The mass analysis was performed with a 4000 QTRAP® mass spectrometer using multiple-ion reaction monitoring (MRM) in the positive mode, with the transition of m/z 325 → m/z 205 for OJT007 and m/z 350 → m/z 101 for voriconazole. The intra- and inter-day precision and accuracy were within ±15%. The mean extraction recovery and the matrix effect were 95.1% and 7.96%, respectively, suggesting no significant matrix interfering with the quantification of the drug in rat plasma. This study was successfully used for the pharmacokinetic evaluation of OJT007 using the rat as an animal model.

scholarly journals Alpha-Tocopherol Metabolites (The Vitamin E Metabolome) and Their Interindividual Variability during Supplementation

Antioxidants ◽  
2021 ◽  
Vol 10 (2) ◽  
pp. 173
Author(s):  
Desirée Bartolini ◽  
Rita Marinelli ◽  
Danilo Giusepponi ◽  
Roberta Galarini ◽  
Carolina Barola ◽  
...  
Keyword(s):  
Vitamin E ◽  
Target Genes ◽  
Interindividual Variability ◽  
Pregnane X Receptor ◽  
Alpha Tocopherol ◽  
Therapeutic Interventions ◽  
Intrinsic Variability ◽  
Blood Leukocytes ◽  
Definition Of ◽  
And Function

The metabolism of α-tocopherol (α-TOH, vitamin E) shows marked interindividual variability, which may influence the response to nutritional and therapeutic interventions with this vitamin. Recently, new metabolomics protocols have fostered the possibility to explore such variability for the different metabolites of α-TOH so far identified in human blood, i.e., the “vitamin E metabolome”, some of which have been reported to promote important biological functions. Such advances prompt the definition of reference values and degree of interindividual variability for these metabolites at different levels of α-TOH intake. To this end, a one-week oral administration protocol with 800 U RRR-α-TOH/day was performed in 17 healthy volunteers, and α-TOH metabolites were measured in plasma before and at the end of the intervention utilizing a recently validated LC-MS/MS procedure; the expression of two target genes of α-TOH with possible a role in the metabolism and function of this vitamin, namely pregnane X receptor (PXR) and the isoform 4F2 of cytochrome P450 (CYP4F2) was assessed by immunoblot in peripheral blood leukocytes. The levels of enzymatic metabolites showed marked interindividual variability that characteristically increased upon supplementation. With the exception of α-CEHC (carboxy-ethyl-hydroxychroman) and the long-chain metabolites M1 and α-13′OH, such variability was found to interfere with the possibility to utilize them as sensitive indicators of α-TOH intake. On the contrary, the free radical-derived metabolite α-tocopheryl quinone significantly correlated with the post-supplementation levels of α-TOH. The supplementation stimulated PXR, but not CYP4F2, expression of leucocytes, and significant correlations were observed between the baseline levels of α-TOH and both the baseline and post-supplementation levels of PXR. These findings provide original analytical and molecular information regarding the human metabolism of α-TOH and its intrinsic variability, which is worth considering in future nutrigenomics and interventions studies.

Combined effects of vitamin E (alpha-tocopherol) and cisplatin on the growth of murine neuroblastoma in vivo

1988 ◽  
Vol 24 (11) ◽  
pp. 1751-1758 ◽  
Author(s):  
Kohji Sue ◽  
Akira Nakagawara ◽  
Shin-Ichi Okuzono ◽  
Takahiko Fukushige ◽  
Keiichi Ikeda
Keyword(s):  
Vitamin E ◽  
Alpha Tocopherol ◽  
Combined Effects ◽  
Murine Neuroblastoma

Cerebrospinal fluid levels of alpha-tocopherol (vitamin E) in Alzheimer's disease

1997 ◽  
Vol 104 (6-7) ◽  
pp. 703-710 ◽  
Author(s):  
F. J. Jiménez-Jiménez ◽  
F. de Bustos ◽  
J. A. Molina ◽  
J. Benito-León ◽  
A. Tallón-Barranco ◽  
...  
Keyword(s):  
Alzheimer’S Disease ◽  
Alzheimer's Disease ◽  
Cerebrospinal Fluid ◽  
Vitamin E ◽  
Alpha Tocopherol ◽  
Cerebrospinal Fluid Levels ◽  
Fluid Levels

scholarly journals Effects of Vitamin E and Vitamin C on Mercury Induced Toxicity in Mice

2013 ◽  
Vol 19 (2) ◽  
pp. 93-100 ◽  
Author(s):  
MA Huq ◽  
MA Awal ◽  
M Mostofa ◽  
A Ghosh ◽  
AR Das
Keyword(s):  
Body Weight ◽  
Vitamin E ◽  
Vitamin C ◽  
Biochemical Parameters ◽  
Hematological Parameters ◽  
Protective Role ◽  
Alpha Tocopherol ◽  
Post Mortem ◽  
Group B ◽  
Vitamin E And C

The present study was undertaken to find out the efficacy of vitamin E and/or vitamin C against mercury (Hg) induced toxicity in mice. Sixty mice were randomly divided into 5 equal groups (n=12). One group of mice (Group A) was kept as control and each of rest four groups (B, C, D and E) were fed with mercuric chloride (HgCl2) in drinking water @ 65 mg/L. In addition to HgCl2 alpha-tocopherol (vitamin E) @ 100 mg/L, ascorbic acid (vitamin C) @ 250 mg/L and combination of vitamin E and vitamin C at same dose were given to the mice of groups C, D and E respectively. All treatments were continued for 28 consecutive days. Four mice of each group were sacrificed on day 1, 14 and 28 and efficacy of vitamin E and vitamin C against Hg induced toxicity were evaluated by observing toxic signs, body weight, hemato-biochemical parameters and postmortem lesions. Mild (++) toxic signs as evident by reduced feed and water intake, salivation, vomiting, excitement, muscle tremor, ataxia, restlessness, incordination and ruffled hair coat were observed from 2nd week (group B) and from 3rd week (group C and D) by intoxication with HgCl2. Significant (P<0.01) reduction of body weight (18.38%) and hematological parameters i.e. TEC (19.88%), TLC (27.89%), Hb content (34.09%) and PCV (9.15%) were observed at day 28 in HgCl2 induced intoxicated mice (group B). At identical period in same group biochemical parameters i.e. AST (46.99%) and ALT (58.72%) increased significantly (p<0.01). Pinpoint hemorrhages throughout the liver and highly (++++) congested kidney was also observed at post mortem (group B). All the parameters i.e. toxic signs, body weight, hemato-biochemical and post mortem lesions were found to be slight (+) or mild (++) and/or improved in rest three groups of mice following treatment with vitamin E, vitamin C and combination of vitamin E and vitamin C. The present study reveals that vitamin E and C have a protective role against Hg poisoning. However, combination of vitamin E and C gave better results.DOI: http://dx.doi.org/10.3329/pa.v19i2.16949 Progress. Agric. 19(2): 93 - 100, 2008

scholarly journals Antigoitrogenic effect of combined supplementation with dl-alpha-tocopherol, ascorbic acid and beta-carotene and of dl-alpha-tocopherol alone in the rat

1998 ◽  
Vol 156 (3) ◽  
pp. 551-561 ◽  
Author(s):  
JF Mutaku ◽  
MC Many ◽  
I Colin ◽  
JF Denef ◽  
MF van den Hove
Keyword(s):  
Endothelial Cells ◽  
Ascorbic Acid ◽  
Vitamin E ◽  
Beta Carotene ◽  
Iodine Content ◽  
Fold Increase ◽  
Alpha Tocopherol ◽  
Free Radical Scavengers ◽  
Rate Of Increase ◽  
Male Wistar Rats

The effects of the vitamins dl-alpha-tocopherol, ascorbic acid and beta-carotene, free radical scavengers and lipid peroxidation inhibitors, were analyzed in male Wistar rats made goitrous by feeding a low iodine diet (< 20 micrograms iodine/kg) and perchlorate (1% in drinking water) for 4, 8, 16, and 32 days. Groups of control or goitrous rats received for at least 16 days before killing a diet containing 0.6% vitamin E (as dl-alpha-tocopherol acetate), 1.2% vitamin C (ascorbic acid) and 0.48% beta-carotene, either simultaneously (vitamin cocktail) or separately. This treatment led to a 5-fold increase of vitamin E in the thyroid gland, a 24-fold increase in the liver and a 3-fold increase in the plasma. In control rats, vitamin cocktail administration increased slightly the thyroid weight with little changes in thyroid function parameters. During iodine deficiency, administration of the vitamin cocktail or vitamin E alone reduced significantly the rate of increase in thyroid weight, and DNA and protein contents, as well as the proportion of [3H]thymidine labeled thyroid follicular cells, but not that of labeled endothelial cells. Plasma tri-iodothyronine, thyroxine, TSH levels, thyroid iodine content and concentration as well as relative volumes of glandular compartments were not modified. The proportion of necrotic cells rose from 0.5% in normal animals to about 2% after 16 days of goiter development. No significant protective effect of the vitamins was observed. These results suggest that these vitamins, particularly vitamin E, modulate one of the regulatory cascades involved in the control of thyroid follicular cell growth, without interfering with the proliferation of endothelial cells.

scholarly journals A SELECTIVE AND SENSITIVE LC-MS/MS METHOD FOR QUANTIFICATION OF FOUR POTENTIAL GENOTOXIC IMPURITIES IN ATAZANAVIR SULFATE DRUG SUBSTANCE IN TRACE LEVEL

2021 ◽  
pp. 137-144
Author(s):  
SIVA JYOTHI N. ◽  
VENKATNARAYANA MUVVALA
Keyword(s):  
Mobile Phase ◽  
Multiple Reaction Monitoring ◽  
Research Work ◽  
Active Pharmaceutical Ingredient ◽  
Drug Substance ◽  
Genotoxic Impurities ◽  
Liquid Chromatography Tandem Mass ◽  
Short Run ◽  
Acquity Uplc ◽  
Atazanavir Sulfate

Objective: The main objective of current research work is to develop and validate a rapid, sensitive and selective liquid chromatography-tandem mass spectrometry (LC-MS/MS) method for the trace analysis of four potential genotoxic impurities in Atazanavir Sulfate drug substance. Methods: LC-MS/MS analysis of four potential genotoxic impurities was done on Acquity UPLC CSH C18 (100 mm × 2.1 mm, 1.7 μm) column. In this method, mobile phase A (10 mM ammonium acetate) mobile phase B (methanol: acetonitrile (90:10, v/v) with gradient run with the flow rate of 0.2 ml/min. The method was developed with the short run time of 13 min. Triple quadrupole mass detector coupled with positive electrospray ionization was used for the quantification of genotoxic impurities in multiple reaction monitoring (MRM) mode. Results: The method was linear in the range of 0.3 ppm to 4.5 ppm for BOC Hydrazine Acid impurity, BOC Epoxide and Keto impurity with a correlation coefficient not less than 0.9994. The accuracy of the method was in the range of 99.26% to 105.71% for all four potential genotoxic impurities (PGIs). No impurities were identified in the Atazanavir Sulfate active pharmaceutical ingredient sample. Conclusion: The proposed method is specific, linear, precise, accurate, robust and stable for the quantification of the four genotoxic impurities at very low levels.

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