scholarly journals Comparative Chemical Profiling and Monacolins Quantification in Red Yeast Rice Dietary Supplements by 1H-NMR and UHPLC-DAD-MS

Molecules ◽  
2020 ◽  
Vol 25 (2) ◽  
pp. 317 ◽  
Author(s):  
Rabab Hachem ◽  
Gaëtan Assemat ◽  
Stéphane Balayssac ◽  
Nathalie Martins-Froment ◽  
Véronique Gilard ◽  
...  

Red yeast rice dietary supplements (RYR DS) are largely sold in Western countries for their cholesterol-lowering/regulating effect due to monacolins, mainly monacolin K (MK), which is, in fact, lovastatin, the first statin drug on the market. 1H-NMR was used as an easy, rapid and accurate method to establish the chemical profiles of 31 RYR DS and to quantify their monacolin contents. Among all the 1H resonances of the monacolins found in RYR, only those of the ethylenic protons of the hexahydronaphthalenic ring at 5.84 and 5.56 ppm are suitable for quantification because they show no overlap with the matrix signals. The total content in monacolins per capsule or tablet determined in 28 DS (the content in 3 DS being below the limit of quantification of the method, ≈ 0.25 mg per unit dose) was close to that measured by UHPLC, as shown by the good linear correlation between the two sets of values (slope 1.00, y-intercept 0.113, r2 0.986). Thirteen of the 31 RYR DS analyzed (i.e., 42%) did not provide label information on the concentration of monacolins and only nine of the 18 formulations with an indication (i.e., 50%) actually contained the declared amount of monacolins.

2020 ◽  
Vol 16 (6) ◽  
pp. 761-767
Author(s):  
Abdul Khader Karakka Kal ◽  
Tajudheen K. Karatt ◽  
Moses Philip ◽  
Samir Meissir ◽  
Jahfar Nalakath

Background: Drug Enforcement Administration confirmed that many manufacturers began adding tetramisole or its individual isomers to cocaine as an adulterant, and believed that tetramisole may augment cocaine’s effects. In recent times, there is an increasing trend in the usage of tetramisole and its individual enantiomer in race sports especially in horse and camel races. So it’s is very much required to confirm the stereochemistry of this illicit drug in the routine race day samples coming to the anti-doping labs in order to avoid legal arguments and challenges to the analytical findings. Methods: The aim of the study was to develop a simple, rapid and accurate method for the chiral separation and determination of enantiomeric mixtures of levamisole and dexamisole using Thermo Q-Exactive High-Resolution Mass Spectrometer. In order to evaluate the suitability of the method for determining the enantiomeric purity of tetramisole, validation studies were also carried out by using equine plasma. Results: The enantio-separation was achieved using the Lux i-cellulose-5 column. Isocratic flow was used with a 1:1 mixture of mobile phase A (10 mM ammonium acetate in water) and mobile phase B (acetonitrile), at a flow rate of 0.6 mL/min. The run time was 8.0 min, and the column temperature was 50°C. Dexamisole eluted at 5.94 min, and levamisole eluted at 6.62 min, giving the R-value of 1.50. The obtained inter-day precisions of dexamisole, levamisole were 3.16% and 2.85%, respectively. The accuracy of dexamisole was in the range of 97.78 to 102.44%, and that for levamisole was 99.16 to 102.82%. The limit of quantification value for both isomers in this method was 0.1 ng/ mL. The method was linear in the range of 0 to 50 ng/mL. Conclusion: Chromatographic separation was achieved using the polysaccharide cellulose chiral column, and the reverse-phase separation approach was found to have the highest potential for successful chiral resolution in LC-MS. Linearity, precision, accuracy, detection limit, recovery, and the matrix effect in equine plasma were determined. Under the optimized conditions, the validated method can be applied for the identification and detection of the tetramisole enantiomers in different sources of illicit drugs of abuse.


Toxins ◽  
2021 ◽  
Vol 13 (7) ◽  
pp. 497
Author(s):  
Magdalena Twarużek ◽  
Iwona Ałtyn ◽  
Robert Kosicki

Citrinin (CIT) is secondary metabolite of filamentous molds. This mycotoxin has nephrotoxic, hepatotoxic, embryocidal, and fetotoxic properties. It is also produced by several species of the three genera Penicillium spp., Aspergillus spp., and Monascus spp., which are used to make red yeast rice (RYR). The material for this study consisted of 15 dietary supplements containing an extract of fermented red rice, available on the Polish market. Samples were extracted using a MeOH–H2O mixture, cleaned-up with an immunoaffinity CitriTest HPLC column, and quantified by HPLC–FLD. None of the analyzed samples contained CIT above the established limit of detection (LOD). Studies on the presence of toxic metabolites in red yeast rice show the importance of regulating this product and of clear information on the label regarding the standardized amounts of monacolin.


2020 ◽  
Vol 0 (0) ◽  
Author(s):  
Hyun Ah Oh ◽  
Min Young Kim ◽  
Yoon Jeong Lee ◽  
Junsoo Lee ◽  
Heon Sang Jeong

Abstract We aimed to develop an efficient process for producing red yeast rice (RYR) with different rice cultivars (Samkwang: used for cooking and Hangaru: used for processing) and amounts of added water (0–100%). Our analyses showed that Hangaru rice had a round starchy form with 18.62% amylose content, and Samkwang rice exhibited an angular starchy form with 15.29% amylose content. The in vitro enzymatic hydrolysis ratio was higher for Hangaru RYR (20.92–24.28%) than for Samakwang RYR (10.97–15.91%) with different amounts of water added. Hangaru RYR showed the highest color value with 60% added water; however, Samkwang RYR highest color value was at 40% added water. The total content of monacolin K was the highest (749.34 mg/kg) for Hangaru RYR treated with 60% added water. These results suggest that Hangaru rice supplemented with 60% water is the most suitable for producing RYR.


2016 ◽  
Vol 8 (3-4) ◽  
pp. 315-318 ◽  
Author(s):  
B.J. Venhuis ◽  
F. Hunsel ◽  
S. Koppel ◽  
P.H.J. Keizers ◽  
S.M.F. Jeurissen ◽  
...  

2017 ◽  
Vol 83 (4) ◽  
pp. 894-908 ◽  
Author(s):  
Gabriela Mazzanti ◽  
Paola Angela Moro ◽  
Emanuel Raschi ◽  
Roberto Da Cas ◽  
Francesca Menniti‐Ippolito

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