The Application of Column Stacking in the Purification of Organic Optoelectronic Materials

In the rapid liquid chromatography, the separation column in series mode is a commonly used method to improve the resolution In the previous application article "Application of multiple separation columns in series to improve the separation degree in the purification of compounds", we have described in detail how the separation column in series can improve the separation degree in principle, and discussed the application of separation column in series in the separation and purification of actual samples In this application case, we take the separation and purification of an organic photoelectric material as an example to demonstrate the practical value of the separation column in series to improve the separation degree In the experimental part, the samples in this paper are the synthetic rough products of organic photoelectric materials, which are provided by an OLED new material research and development company For the application of sepabean ® machine with sepaflash ® series separation column in the rapid purification and preparation of organic photoelectric materials, please refer to another application case of sepabean ® machine rapid preparation chromatographic system in the field of organic photoelectric materials published before Firstly, the samples were analyzed by TLC The samples were spotted on the TLC plate and then placed in the developing cylinder The developing agent was n-hexane / ethyl acetate It can be seen from the observation of TLC display board (as shown in Figure 1) that the purity of the sample is not high, two obvious relatively thick impurity points can be seen, and the distance between the impurity point and the corresponding point of the target compound is very close, the separation degree is not high, and the subsequent separation and purification is difficult Fig 1 TLC schematic diagram (left part) and TLC spot plate results (right part) of the sample Researchers of Santai science and Technology Application Technology Research Center conducted the separation and purification experiment of the sample using sepafflash ® series positive phase separation column In order to improve the separation of samples, the researchers used the separation column in series mode First, they tried the sepafflash ® standard fast separation column After two separation columns of the same specification were connected in series, then a solid sample column was connected at the upper end of the separation column Take 100mg of the sample and dissolve it in DCM, mix it with 1g of silica gel, spin dry the sample solvent and place the solid sample in the solid upper sample column The parameters of flash preparation and purification of samples are shown in Table 1 Table 1 Sepabean ® machine 2 chromatographic column 12 g sepaflash ® standard fast separation column (amorphous silica gel, 40-63 μ m, 60 μ m, order No.: s-8101-0012) 12 g sepaflash ® high efficiency series fast separation column (high load spherical silica gel, 25 μ m, 50 μ m, Order No.: sw-2102-012-sp (H)) detection wavelength: 220 nm; mobile phase solvent A: n-hexane; solvent B: ethyl acetate flow rate: 15 ml / min injection volume: 100 mg crude product elution gradient time (min); solvent B (%) 0.30.5 43.5 55 The results of 9 56 100 65 100 and the separation spectrum of the sample under the condition of two standard fast separation columns in series are shown in Figure 2 Figure 2 Analysis of the preparation and separation spectrum (right part) of the sample under the condition that two standard type rapid separation columns are used in series (left part) Figure 2 shows that the target compounds and impurities fail to reach the baseline separation, indicating that the standard type rapid separation columns are not used in series to obtain sufficient resolution In response to this situation, the researchers next tried the sepaflash ® efficient series fast separation column with smaller particle size Two sepaflash ® high efficiency series fast separation columns of the same specification are connected in series, and other experimental conditions remain unchanged Under this condition, the sample is separated and purified, and the separation spectrum is shown in Figure 3 Fig 3 Analysis of the preparation and separation spectrum of the sample under the condition of two high-efficiency rapid separation columns in series (left part) Fig 3 shows that the target compound and impurities have been separated by baseline, and the separation degree is high, indicating that after replacing the high-efficiency series rapid separation columns, the column series mode has achieved the separation degree meeting the purification requirements To further verify the purification results, samples were taken from the collection components corresponding to the target compounds and impurities for TLC spot plate detection, and the results are shown in Figure 4 It can be seen from Fig 4 that the target compounds and impurities are well separated and purified, which can be used for further research Figure 4 The TLC spot plate results of the original samples and the components collected after purification have various specifications for the sepaflash ® high efficiency series rapid separation column products launched by Santai Technology (see Table 2) Table 2 Parameters of sepaflash ® high-efficiency series rapid separation column (packing: high capacityphysical silica, 25 μ m, 50 μ m) item number column size flow rate (ml / min) max.pressure (PSI / bar) sw-2102-004-sp (H) 4 g 15-30 400 / 27.5 sw-2102-012-sp (H) 12 g 25-50 400 / 27.5
SW-2102-025-SP(H)
25 g
25-50
400/27.5
SW-2102-040-SP(H)
40 g
30-60
400/27.5
SW-2102-080-SP(H)
80 g
40-80
350/24.0
SW-2102-120-SP(H)
120 g
45-90
300/20.7
SW-2102-220-SP(H)
220 g
60-120
300/20.7
SW-2102-330-SP(H)
330 g 60-120 250 / 17.2 to learn more about the detailed specifications of sepabean ® machine, or the ordering information of flash purification column, please visit CBG online store: https://store.chembiango.cn/.