Development of integrated equipment for automatic sampling and distillate collection

doi:10.3724/SP.J.1123.2024.12005

Abstract

Abstract:

Preparative chromatography plays an important separation and purification role in the pharmaceutical， chemical， and food industries. New preparative chromatography equipment that integrates automatic sampling and fraction-collecting functions was developed to improve separation efficiency and ease of use， and to meet the separation-efficiency and collection-accuracy needs of modern industry.The design concept and working principles of the device are introduced in detail. The developed equipment significantly improves the injection rate and reduces human operating errors through advanced automation technology， leading to an experimental process that is entirely more scientific and efficient. At the same time， the fraction-collection system was optimized such that it can flexibly adjust to various application requirements， thereby ensuring the highest purities and recoveries of the collected target ingredients. This innovative equipment uses a high-speed servo motor to independently drive the X-， Y-， and Z-axes of the instrument tray in order to realize high-speed sampling and collection actions at any position within the scope of the set tray， while synchronously sampling and collecting. A control circuit was used to calibrate the sampling and collection positions to ensure accuracy and that the device is compatible with a variety of sample-tray specifications to meet the preparation requirements of a wide 1–200 mL/min flow range. The developed equipment was used to separate and purify samples of stevioside and rebaudioside A， and exhibited excellent performance， including fast separation， stable output， and accurate collection. The equipment is capable of realizing synchronous sample-collection functions， thereby providing a stable and reliable separation and purification option for a wide range of industries.

Key words: automatic samples, fraction collection, preparative chromatography, equipment development

CLC Number:

O658

ZHOU Xinying, KONG Weiheng, YU Dexiu, LI Tangyi, MA Zhou, YI Xin, WANG Fenglin, LI Tong. Development of integrated equipment for automatic sampling and distillate collection[J]. Chinese Journal of Chromatography, 2025, 43(7): 830-835.

Figures/Tables 9

Fig. 1 Design roadmap

Fig. 2 Design schematic diagram

Fig. 3 Schematic diagram of the pallet floor

Fig. 4 Mechanical structure odesign drawing1. X-axis； 2. Y-axis； 3. Z-axis； 4. S-axis； 5. injection valve； 6. collecting valve； 7. syringe； 8. sample tray； 9. peristaltic pump； 10. pallet floor； 11. cleaning body； 12. cleaning bottle.

Fig. 5 Pallet typesa. 96 holes； b. 75 holes； c. 70 holes； d. 30 holes； e. 3 holes； f. double 96-well.

Fig. 6 Principle of fraction collectionCOM： common； NO： normally open； NC： normally closed； s1： the signal strength set in the method； t1： the start collection time set in the method for sample 1； t2： the end collection time set in the method for sample 1， and the start collection time set in the method for sample 2； t3： the end collection time set in the method for sample 2； ta： the actual start collection time for sample 1； tb： the actual end collection time for sample 1； tc： the actual start collection time for sample 2； td： the actual end collection time for sample 2.

Table 1 Sampling error

Injection volume/mL	Actual volume/mL	Sampling error/%
1	1.0009	0.56
2	2.0066	0.33
10	9.9363	-0.64

Table 2 Stevioside and rebaudioside A （RA） purity results

Compound	Contents/（mg/mL）		Purity/%
Compound	Actual	Test	Purity/%
Stevioside	1.00	0.99	95.32
RA	0.96	0.95	93.38

Table 3 Reliability evaluation result

MTBF/h	Sampling error （n=7）/%	Collection location
0	-0.64	accurate
3000	-0.57	accurate

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