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采用光电二极管阵列检测器和质谱联用的同步高效液相色谱法测定红曲米中的桔霉素、红曲素、红曲黄素以及莫纳可林K的内酯形式和酸形式。

Synchronous high-performance liquid chromatography with a photodiode array detector and mass spectrometry for the determination of citrinin, monascin, ankaflavin, and the lactone and acid forms of monacolin K in red mold rice.

作者信息

Wu Cheng-Lun, Kuo Yao-Haur, Lee Chun-Lin, Hsu Ya-Wen, Pan Tzu-Ming

机构信息

Sunway Biotechnology Co., R&D Division, Taipei, Taiwan, Republic of China.

出版信息

J AOAC Int. 2011 Jan-Feb;94(1):179-90.

Abstract

The Monascus fermentation product red mold rice (RMR) has been found to contain the cholesterol-lowering agent monacolin K (MK) in both its lactone (MKL) and acid (MKA) forms and the mycotoxin citrinin (CT). The yellow pigments in RMR, namely, monascin (MS) and ankaflavin (AK), have been reported to exhibit antimetastatic and antiangiogenic activities. Currently, MK and these yellow pigments are usually detected in RMR by different analytical methods that are inconvenient, expensive, and time-consuming. The goal of this study was to establish a rapid, synchronous analytical method for determination of the MKA, MKL, MS, AK, and CT levels in RMR. MKA, MKL, MS, AK, and CT were extracted by the same extraction method, then separated by RP-HPLC with a C18 column. The effluent from the column was passed through a photodiode array detector and then introduced directly into a fluorescence detector. The results showed that high recovery rates of MKA, MKL, MS, AK, and CT are possible if RMR powder is extracted with 75% ethanol (10 mL) at 80 degrees C for 30 min. With regard to the optimal conditions of the HPLC, the peaks of MKA, MKL, MS, AK, and CT can be clearly separated from any noise peaks by isocratic elution with a mobile phase comprising 0.05% trifluoroacetic acid in acetonitrile-water (62.5 + 37.5, v/v).

摘要

红曲霉菌发酵产物红曲米(RMR)已被发现含有降胆固醇剂莫纳可林K(MK)的内酯形式(MKL)和酸形式(MKA)以及霉菌毒素桔霉素(CT)。据报道,RMR中的黄色色素,即红曲素(MS)和安卡黄素(AK),具有抗转移和抗血管生成活性。目前,通常采用不同的分析方法来检测RMR中的MK和这些黄色色素,这些方法不方便、昂贵且耗时。本研究的目的是建立一种快速、同步的分析方法,用于测定RMR中MKA、MKL、MS、AK和CT的含量。MKA、MKL、MS、AK和CT采用相同的提取方法进行提取,然后用C18柱通过反相高效液相色谱法(RP-HPLC)进行分离。柱流出物通过光电二极管阵列检测器,然后直接引入荧光检测器。结果表明,如果将RMR粉末在80℃下用75%乙醇(10 mL)提取30 min,MKA、MKL、MS、AK和CT的回收率较高。关于HPLC的最佳条件,通过用包含0.05%三氟乙酸的乙腈-水(62.5 + 37.5,v/v)的流动相进行等度洗脱,可以将MKA、MKL、MS、AK和CT的峰与任何噪声峰清晰分离。

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