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目的:采用近红外在线监测技术,建立红参提取液定量预测模型,并用高效液相色谱测定4种人参皂苷的含量。方法:利用近红外光谱法在线监测提取过程,近红外光谱仪扫描方式为光纤透射扫描,光谱范围1 000~2 500 cm-1,分辨率1cm-1,以空气为空白,扫描次数16次,1倍增益;采用高效液相色谱法测定红参提取液中人参皂苷Rg1、Ro、Rb1、Rc的含量,使用Phenomenex Luna C18色谱柱(4.6 mm×250 mm,5μm),以0.1%乙酸铵水溶液-乙腈(80∶20)为流动相梯度洗脱,流速1.0m L·min-1,柱温30℃,检测波长207 nm,外标法定量。并对检测结果进行比较研究。结果:红参提取液4个人参皂苷含量6次提取过程均在近2 h内达到平衡,不同批红参提取液中人参皂苷含量变化基本相同,指数趋势线变化基本相同,均渐低渐缓,且相同提取时间内各成分含量相互间差异不大。结论:在线近红外光谱技术经方法学验证,可用于监控红参提取工艺。
OBJECTIVE: To establish a quantitative prediction model of red ginseng extract by near-infrared on-line monitoring technique and determine the contents of four ginsenosides by high performance liquid chromatography. Methods: The extraction process was monitored online by near infrared spectroscopy (FTIR). The near infrared spectroscopy (FTIR) scanning method was fiber transmission scanning with the spectral range of 1 000-2 500 cm -1 and the resolution of 1 cm -1. The air was blank and the number of scanning times was 16 Fold increase; the content of ginsenoside Rg1, Ro, Rb1 and Rc in red ginseng extract was determined by HPLC. The residue was purified on a Phenomenex Luna C18 column (4.6 mm × 250 mm, 5 μm) with 0.1% Acetonitrile (80:20) was used as mobile phase gradient elution at a flow rate of 1.0 mL min-1. The column temperature was 30 ℃ and the detection wavelength was set at 207 nm. And the test results were compared. Results: The extraction of 4 ginsenosides in the red ginseng extract reached equilibrium within two hours. The contents of ginsenosides in different ginseng extracts were basically the same, and the changes of the index trend lines were basically the same, all gradually decreasing , And the content of each component within the same extraction time is not different from each other. Conclusion: On-line NIR spectroscopy is validated by methodology and can be used to monitor the red ginseng extraction process.