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首页> 外文期刊>Separation and Purification Technology >A feasible scaling-up separation of platycosides from Platycodi Radix: From analytical to semi-preparative high performance liquid chromatography coupling with a post-separation flash freezing treatment to obtain highly unstable components
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A feasible scaling-up separation of platycosides from Platycodi Radix: From analytical to semi-preparative high performance liquid chromatography coupling with a post-separation flash freezing treatment to obtain highly unstable components

机译：可行的按比例放大从Platycodi Radix分离出板载糖苷的方法：从分析型到半制备型高效液相色谱，再加上快速分离后冷冻处理，可获得高度不稳定的组分

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摘要

A method of using semi-preparative HPLC coupling with a post-HPLC flash freezing treatment to separate platycosides from Platycodi Radix is developed. Nine platycosides including unstable acetyl platycosides were separated from Platycodi Radix by semi-preparative HPLC. Separation variables of flow rate and loading amount of sample were linearly scaled up from analytical HPLC to semi-preparative HPLC. Variables of semi-preparative HPLC separation including flow rate and loading amount of sample were calculated as 29.8 mL/min and 297.7 mg, respectively. Under the optimized conditions of separation, nine platycosides were simultaneously separated on semi-preparative scale within 1 h. Separation resolutions of the peaks of platycosides were all above 0.85, of which seven platycosides were separated with resolutions above 1.00. With regards to sample pretreatment before chromatography separation, we propose a post-HPLC treatment to the unstable compounds. A post-HPLC treatment by using liquid nitrogen to flash freeze the eluent fractions from semi-preparative HPLC was used to stop the unstable platycosides transformation. By freezing treatment, the pure unstable acetyl platycosides were obtained without transformation. This was the first time that unstable acetyl platycosides were simultaneously separated by preparative HPLC. This method is fast and efficient to separate platycosides from Platycodi Radix, especially for purifying unstable platycosides. (C) 2016 Elsevier B.V. All rights reserved.
机译：开发了一种将半制备型HPLC与HPLC后快速冷冻处理结合使用，以从Platycodi Radix中分离板状苷的方法。通过半制备型HPLC从Platycodi Radix分离出包括不稳定的乙酰基platycosides在内的9种platycoside。样品流速和上样量的分离变量从分析型HPLC线性放大到半制备型HPLC。半制备型HPLC分离变量包括样品的流速和上样量分别计算为29.8 mL / min和297.7 mg。在最佳分离条件下，在1 h内以半制备规模同时分离了9种桔梗。桔梗各峰的分离度均在0.85以上，其中分离出7种桔梗，其分度在1.00以上。关于色谱分离之前的样品预处理，我们建议对不稳定的化合物进行HPLC后处理。通过使用液氮使半制备型HPLC的洗脱液馏分快速冷冻的HPLC后处理用于终止不稳定的板状肽的转化。通过冷冻处理，获得了纯的不稳定的乙酰铂类，没有转化。这是首次通过制备型HPLC同时分离不稳定的乙酰铂盐。该方法快速有效地从Platycodi Radix中分离出板状苷，特别是用于纯化不稳定的板状苷。 （C）2016 Elsevier B.V.保留所有权利。

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