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改进了高效液相色谱法检测莫纳可林K(Monacolin K,MK)的流动相,主要优化了流动相中有机相的种类、浓度以及磷酸添加量,并考察了流动相对分析红曲样品中MK含量及MK同系物的影响。结果表明,与甲醇相比,以不同体积分数的乙腈作为流动相中的有机相时对MK的峰面积影响较小,且酸式MK(Monacolin K in acid form,MKA)及内酯式MK(Monacolin K in lactone form,MKL)分离度高。当流动相中乙腈体积分数为60%时,MKA与MKL的分离度可达6.72,利于与MKA及MKL极性相近的MK同系物分析。0.5%磷酸添加量在2%~5%范围内对MK的峰面积及保留时间均无显著影响(p>0.05)。与现有行业标准(QB/T 2847—2007)相比,流动相中磷酸添加量越高,MKA测定结果相对越低。当流动相为乙腈、水、0.5%磷酸体积比60∶37∶3时,可在准确测定MK含量的基础上有效分离MK同系物,且检测时长可控制在30 min内。试验可为MK指纹图谱建立及功能红曲的快速鉴伪提供新的思路。
The mobile phase of Monacolin K (MK) was improved by high performance liquid chromatography (HPLC). The type and concentration of organic phase in the mobile phase and the amount of phosphoric acid were optimized. MK content and MK homologues. The results showed that the effect of different volume fractions of acetonitrile on the mobile phase was smaller than that of methanol, and the peak area of MK was smaller than that of methanol. The acidity of MK (MKA) and lactone MK Monacolin K in lactone form, MKL) High resolution. When the volume fraction of acetonitrile in the mobile phase was 60%, the resolution of MKA to MKL was 6.72, which favored the analysis of MK homologues with similar polarities to MKA and MKL. The addition of 0.5% phosphoric acid had no significant effect on the peak area and the retention time of MK in the range of 2% ~ 5% (p> 0.05). Compared to the current industry standard (QB / T 2847-2007), the higher the amount of phosphoric acid in the mobile phase, the lower the MKA measurement. When the mobile phase consisted of acetonitrile, water and 0.5% phosphoric acid with a volume ratio of 60:37:3, the MK homologues could be effectively separated on the basis of accurate determination of the content of MK, and the test duration could be controlled within 30 min. The experiment can provide new ideas for the establishment of MK fingerprinting and the rapid identification of functional Monascus.