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| Determination of residual ethanol and acetone in refined polysaccharide from pneumococcal serotype 6B by headspace gas chromatography |
| QI Qiuhuan HUANG Chunhua ZHENG Xuexue HAN Fei WANG Cuijie LI Xiangqun |
Beijing Minhai Biotechnology Co., Ltd., Beijing 102600, China
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Abstract Objective To establish a headspace gas chromatography method for the determination of residual ethanol and acetone in the refined polysaccharide from pneumococcal serotype 6B. Methods The residual amounts of ethanol and acetone in the refined polysaccharide from pneumococcal serotype 6B by Beijing Minhai Biotechnology Co., Ltd. were determined by headspace gas chromatography with water as solvent. The chromatographic conditions were as follows: DB-624 capillary column (30 m × 0.25 mm, 1.80 μm); the flow rate of carrier gas chromatographic column was 3.00 ml/min, and the split ratio was 10∶1. The initial column temperature was maintained at 40℃ for 2 min, then raised to 80℃ at a rate of 5℃ per minute for 4 min; and raised to 200℃ at a rate of 20℃ per minute for 2 min; The detector temperature was 240℃. The temperature of thermostatic furnace was 80℃ and the equilibrium time was 30 min. The system applicability, specificity, detection limit, quantitative limit, linear range, accuracy, repeatability, and reproducibility of the method were verified. Results The theoretical plate number of ethanol and acetone was≥5 000, and the resolution was ≥1.5. Phenol had no interference to the residue of ethanol and acetone. The limit of detection of ethanol was 0.199 μg/ml, and the limit of quantitation was 0.596 μg/ml. The detection limit of acetone was 0.051 μg/ml, and the limit of quantitation was 0.152 μg/ml. The linear equation of ethanol was Y=2 276.471 86X-265.405 07, r=0.999 99, and the linear range was 0.090 - 30.000 μg/ml. The linear equation of acetone was Y=7 790.898 42X+4 216.806 23, r= 0.998 13, and the linear range was 0.120-40.000 μg/ml. The accuracy recovery rate of from pneu- mococcal serotype 6B was 86.20 %-100.66 % for ethanol and 82.89 %-91.42 % for acetone. The repeatability RSD was 2.3 % for ethanol and 5.5 % for acetone. The RSD of intermediate precision was 7.2% for ethanol and 4.2% for acetone. The residual range of ethanol in 9 batches of samples was not detected to 6.184 μg/ml, and the residual range of acetone was not detected to 10.475 μg/ml. Conclusion The method of headspace gas chromatography for the determination of ethanol and acetone residues in refined polysaccharide from pheumococcal serotype 6B has good system suitability, accuracy, precision and linearity. The method is rapid, simple and reliable. It can be used for the determination of ethanol and acetone residues in refined polysaccharide from pheumococcal serotype 6B.
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