Bioanalytical Method Development and Validation Study of Neuroprotective Extract of Kashmiri Saffron Using Ultra-Fast Liquid Chromatography-Tandem Mass Spectrometry (UFLC-MS/MS): In Vivo Pharmacokinetics of Apocarotenoids and Carotenoids

Girme, Aboli; Pawar, Sandeep; Ghule, Chetana; Shengule, Sushant; Saste, Ganesh; Balasubramaniam, Arun; Deshmukh, Amol S.; Hingorani, Lal

doi:10.3390/molecules26061815

Cited by 17 publications

(11 citation statements)

References 47 publications

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“…Saffron is the main natural source of crocins (crocetin esters), which are water-soluble carotenoid derivatives constituting in a general content ranges between 16–28% in dried stigmas [ 25 ]. Because of its rarity and extremely high price of saffron, seeking alternative sources, i.e., the agricultural wastes have extremely high potential value.…”

Section: Resultsmentioning

confidence: 99%

High-Purity Preparation of Enzyme Transformed Trans-Crocetin Reclaimed from Gardenia Fruit Waste

Chyau

Chiu

Hsieh

et al. 2022

Plants

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The recovery of physiologically bioactive ingredients from agricultural wastes as an abundant and low-cost source for the production of high value-added mutraceuticlas has been recognized and supported for the commercial interests and sustainable managements. In the extraction of geniposide for the development of natural food colorants from the dried fruits of Gardenia jasminoides Rubiaceae, the gardenia fruit waste (GFW) still remaining 0.86% (w/w) of crocins has always been discarded without any further treatments Until now, there was no simple and effective protocol for high-purity trans-crocein (TC) preparation without the coexistence of non-biologically active cis-crocein from GFW. We proposed an effective process to obtain the compound as follows. Crocins were extracted firstly by 50% of ethanol in the highest yield of 8.61 mg/g (w/w) from GFW. After the HPD-100 column fractionation in the collecting of crocins, the conversion ratio of 75% of crocins to crocetins can be obtained from the commercial available enzyme- Celluclast® 1.5 L. The crocins hydrolyzed products, were then separated through the HPD-100 resin adsorption and finally purified with the centrifugal partition chromatography (CPC) in single-step to obtain TC in a purity of 96.76 ± 0.17%. Conclusively, the effective enzyme transformation and purification co-operated with CPC technologies on crocins resulted in a high purity product of TC may be highly application in the commercial production.

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Section: Resultsmentioning

confidence: 99%

High-Purity Preparation of Enzyme Transformed Trans-Crocetin Reclaimed from Gardenia Fruit Waste

Chyau

Chiu

Hsieh

et al. 2022

Plants

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“…The separated plasma samples were transferred into Eppendorf tubes and stored at −80 °C in a deep freezer until analysis. Ten pharmacokinetic parameters were determined using PK solver 2.0, USA [ 45 , 46 , 47 ]. The maximum observed concentration (C max ) and maximum observed time (T max ) were calculated directly from the experimental results.…”

Section: Methodsmentioning

confidence: 99%

Pharmacokinetic Study of Withanosides and Withanolides from Withania somnifera Using Ultra-High Performance Liquid Chromatography-Tandem Mass Spectrometry (UHPLC-MS/MS)

et al. 2022

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Withania somnifera is a traditional Indian herb described under the ‘Rasayana’ class in Ayurveda, which gained immense popularity as a dietary supplement in the USA, Europe, Asia, and the Indian domestic market. Despite enormous research on the pharmacological effect of withanosides and withanolides, bioanalytical method development and pharmacokinetics remained challenging and unexplored for these constituents due to isomeric and isobaric characteristics. In current research work, molecular descriptors, pharmacokinetic, and toxicity prediction (ADMET) of these constituents were performed using Molinspiration and admetSAR tools. A rapid, selective, and reproducible bioanalytical method was developed and validated for seven withanosides and withanolides as per USFDA/EMA guidelines, further applied to determine pharmacokinetic parameters of Withania somnifera root extract (WSE) constituents in male Sprague Dawley rats at a dose of 500 mg/kg. Additionally, an ex vivo permeability study was carried out to explore the absorption pattern of withanosides and withanolides from the intestinal lumen. In silico, ADMET revealed oral bioavailability of withanosides and withanolides following Lipinski’s rules of five with significant absorption from the gastrointestinal tract and the ability to cross the blood-brain barrier. Upon oral administration of WSE, Cmax was found to be 13.833 ± 3.727, 124.415 ± 64.932, 57.536 ± 7.523, and 7.283 ± 3.341 ng/mL for withanoside IV, withaferin A, 12-Deoxy-withastramonolide, and withanolide A, respectively, with Tmax of 0.750 ± 0.000, 0.250 ± 0.000, 0.291 ± 0.102, and 0.333 ± 0.129 h. Moreover, at a given dose, withanoside V, withanolide B, and withanone were detected in plasma; however, the concentration of these constituents was found below LLOQ. Thus, these four major withanoside and withanolides were quantified in plasma supported by ex vivo permeation data exhibiting a time-dependent absorption of withanosides and withanolides across the intestinal barrier. These composite findings provide insights to design a clinical trial of WSE as a potent nutraceutical.

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“…Although crocins occur naturally in abundance, however, it undergoes bioactivation in the biological system to produce lipophilic crocetin (aglycone) that crosses the blood–brain barrier. We have previously shown that crocin, trans -crocetin, and safranal display an anti-Alzheimer effect by either Aβ-clearance or blocking neuroinflammation. ,, Furthermore, the recent pharmacokinetic study revealed the presence of these crocins and crocetin, with picrocrocin and safranal in vivo after oral administration of CSE, demonstrating its role as a promising botanical lead . Thus, in the present study, we have carried out quantification studies for these crocins and crocetin.…”

Section: Introductionmentioning

confidence: 75%

“…Different solvents and their combination were applied to the samples (CSE) for maximum and consistent separation with the extraction of targeted analytes ( 1–7 ) (Figure ). The extraction solvents were chosen based on the literature and the solubility of targeted apocarotenoids. ,− The solvent system 1 [dimethyl sulfoxide (DMSO)/methanol, 20:80 v / v ], solvent system 2 (water/methanol, 50:50 v / v ), solvent system 3 (water), solvent system 4 (methanol), and solvent system 5 (DMSO) were optimized with ultrasonication-assisted extraction with temperature (25–30 °C) followed by HPLC analysis. A simple liquid–liquid extraction technique of solvent system 1 (DMSO: methanol, 20:80 v / v ) was finalized for further analysis based on stability, the maximum response of targeted analytes with reproducible results compared to other solvents (Figures S1–S3, Supporting Information).…”

Section: Results and Discussionmentioning

confidence: 99%

Quantitative Determination and Characterization of a Kashmir Saffron (Crocus sativus L.)-Based Botanical Supplement Using Single-Laboratory Validation Study by HPLC-PDA with LC–MS/MS and HPTLC Investigations

et al. 2021

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Food ingredients hold a higher nutritional value as a botanical supplement playing a vital role in modifying and maintaining the physiological conditions that improve human health benefits. The Kashmir saffron ( Crocus sativus L; KCS) obtained from dried stigmas is known for its aroma precursors and apocarotenoid derivatives, imparting a wide range of medicinal values and therapeutic benefits. In the present study, a simultaneous determination of apocarotenoids and flavonoids in stigma-based botanical supplements was carried out using analytical investigations. The high-performance thin-layer chromatography-based qualitative analysis of the raw material (stigmas, stamens, and tepals) and stigma extract has been carried out to identify apocarotenoids and flavonoids. The rapid HPLC-PDA method for the simultaneous quantification of KCS apocarotenoids was robust, precise (<5.0%), linear ( R 2 > 0.99), and accurate (80–110%) as per the single-laboratory validation data. Furthermore, the combined-expanded uncertainty (95%; K = 2) was calculated and found as 0.0035–0.007% (<5.0%) as per the EURACHEM guide for this HPLC analysis. Additionally, an untargeted identification of 36 compounds in the botanical supplement was based on the elution order, UV–vis spectra, mass fragmentation pattern, and standards by ESI-MS/MS analysis with comprehensive chromatographic fingerprinting. Thus, these analytical approaches enable a composite profile of the stigma-based extract as a potential supplement for human health benefits.

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Bioanalytical Method Development and Validation Study of Neuroprotective Extract of Kashmiri Saffron Using Ultra-Fast Liquid Chromatography-Tandem Mass Spectrometry (UFLC-MS/MS): In Vivo Pharmacokinetics of Apocarotenoids and Carotenoids

Cited by 17 publications

References 47 publications

High-Purity Preparation of Enzyme Transformed Trans-Crocetin Reclaimed from Gardenia Fruit Waste

High-Purity Preparation of Enzyme Transformed Trans-Crocetin Reclaimed from Gardenia Fruit Waste

Pharmacokinetic Study of Withanosides and Withanolides from Withania somnifera Using Ultra-High Performance Liquid Chromatography-Tandem Mass Spectrometry (UHPLC-MS/MS)

Quantitative Determination and Characterization of a Kashmir Saffron (Crocus sativus L.)-Based Botanical Supplement Using Single-Laboratory Validation Study by HPLC-PDA with LC–MS/MS and HPTLC Investigations

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