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

机译:通过1H-NMR和UHPLC-DAD-MS对红曲米膳食补充剂中的化学分析和莫纳可林进行定量比较

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摘要

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. H-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 H 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, r 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.
机译:红曲米膳食补充剂(RYR DS)在西方国家因其降胆固醇/调节作用而在西方国家大量销售,这主要归功于莫纳可林素,主要是莫纳可林K(MK),事实上,莫纳可林K(洛伐他汀)是市场上第一种他汀类药物。 H-NMR是一种简便,快速,准确的方法,用于建立31 RYR DS的化学谱图并定量其莫纳可林含量。在RYR中发现的monacolins的所有H共振中,只有六氢萘环的烯键质子在5.84和5.56 ppm处的那些H共振适合于定量,因为它们与基质信号没有重叠。线性良好显示,在28 DS中测定的每个胶囊或片剂中莫纳可林的总含量(3 DS中的含量低于该方法的定量限,≈每单位剂量0.25 mg)接近于UHPLC测定的含量。两组值之间的相关性(斜率1.00,y轴截距0.113,r 0.986)。在31个RYR DS中,有13个(即42%)未提供有关莫那可林浓度的标签信息,并且在18种配方中有指示的制剂(即50%)中实际上只有9个声明了莫那可林的含量。

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