Ilok-sl series integrated column for sample separation -- a new scheme for separation and purification of complex intermediates

In the daily work of synthesis researchers, it is a routine operation for the application technology research center to separate and purify the synthesized intermediates Choosing the right way to sample has an important influence on the purity and yield of the final product For many compound samples, their own physical and chemical properties determine which method is suitable to use in the purification process: liquid injection or solid injection If the sample itself is a liquid, the method of liquid injection can be used directly; if the sample itself is a solid, it needs to use a suitable solvent to dissolve it and then sample, generally using a solvent with similar polarity and mobile phase to dissolve the sample However, some special samples are not easy to dissolve, so it is often necessary to use strong polar solvent to dissolve them At this time, if the method of direct injection of liquid is adopted, the solvent effect is easy to appear, and the phenomena such as peak broadening, tailing before peak and so on are shown in the preparation of chromatogram The solution for this phenomenon is: after dissolving the sample with strong polar solvent, mix the sample with the subsequent separation filler, then remove the solvent by rotary evaporation and sample on the solid, so as to effectively improve the effect of separation and purification In the scheme of solid sample loading, the usual method is to connect a sample loading empty column through the adapter before the separation column, and the empty column is used to add the sample to complete the sample mixing treatment The disadvantage of this method is that the dead volume of the empty column and the adapter itself is easy to cause the diffusion of the sample, thus reducing the separation efficiency In view of the above problems, Santai technology has launched ilok-sl series integrated column for sample loading and separation 15% space is reserved at the front of the column for solid sample loading, so as to minimize the dead volume between the sample and the separation packing and ensure the best separation effect Next, the purification of a synthetic intermediate is introduced in detail Experiment part 1 Sample information the sample in this case is the intermediate of a certain synthesis reaction, with a total of about 20 g the final synthesis reaction formula is shown in Figure 1 Figure 1 Chemical reaction formula of synthetic intermediate sample 2 Through TLC spot plate analysis (as shown in Figure 2), it is found that there is a very close impurity point near the corresponding spot of the target compound, which may cause great obstacles to the subsequent separation and purification Attention must be paid when selecting separation conditions Figure 2 Sample spot results on TLC plate 3 Flash preparation and purification of sample calculate Rf value of target compound and main impurity spot according to TLC spot information, then input the above data (as shown in Figure 3) on the corresponding page of iPad terminal control software of sepabean ® machine t, and the control software can automatically recommend optimized elution gradient Fig 3 the Flash preparation experimental parameters of the TLC information sample input into the SepaBean control software are shown in Table 1, and the Flash preparation purification spectrum is shown in Fig 4 Table 1 Sepabean ® machine t column 330g ilok-sl positive phase separation column (amorphous silica gel, 40-63 μ m, 60 μ m, Order No.: sl-8101-330) detection wavelength 254 nm; 280 nm mobile phase solvent A: n-hexane; solvent B: ethyl acetate flow rate 80 ml / min injection volume 20 g elution gradient column volume (CV) solvent B (%) 0.535 8 40 9 40 13 45 15 45 20 55 24 55 Figure 4 After TLC dot plate analysis, the impurities in the prepared target product have been completely removed, which can be used in further experiments Features of ilok-sl series sample separation integrated column: 1) easy to remove screw cover design, easy sample loading and rapid separation; 2) ten million pieces of separation column production experience, to ensure high quality filling effect 3) Built in injection mode, reduce sample diffusion, show better separation effect, symmetrical peak type, excellent resolution Sepabean ® machine t produced by Santai technology, together with ilok-sl series sample separation integrated column, can provide users with fast and efficient sample preparation and purification solutions, and help laboratory researchers easily complete various sample purification tasks For ordering information of ilok-sl series, please refer to the following link: https://store.chembergo.cn/goods/pub/detail? Id = 140 To learn more about the detailed specifications of sepabean ® machine t, or the ordering information of the flash purification column used with it, please visit CBG online store.