麦冬提取工艺近红外光谱与液相色谱比较研究

目的:采用近红外在线监测技术建立麦冬提取液定量模型,同时用高效液相色谱测定麦冬3种成分的含量。方法:利用近红外光谱法在线监测提取过程,光谱仪扫描方式为光纤透射扫描,光谱范围1 000~2 500 cm,分辨率1 cm,以空气为空白,扫描次数16次,1倍增益;采用HPLC法测定麦冬提取液中甲基麦冬黄烷酮A、甲基麦冬黄烷酮B和亚油酸的含量,使用Grace Alltima C_(18)(4.6 mm×250 mm,5μm)色谱柱,以乙腈为流动相B,以1 mmol/L乙酸铵水溶液为流动相A梯度洗脱,流速1.0 m L/min,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:麦冬提取液3个成分含量2次提取过程中均在近2小时内达到平衡,不同批麦冬提取液中3个成分含量变化基本相同且相互之间差异不大。结论:在线近红外光谱技术经方法学验证,可用于监控麦冬提取工艺。

Study on MaiDong Extraction Technology of Near-infrared Spectroscopy and Liquid Chromatography

Objective:To build quantitative model of MaiDong[Ophiopogon japonicus (Linn. f.) Ker-Gawl.] extracting solution by using near-infrared monitoring technology, and to measure three components of MaiDong by using liquid chromatography (LC). Methods:Extraction process was monitored by near-infrared spectrometry, the scanning mode of spectrometer was fiber transmission scan, the ranges of spectrum were from 1000 to 2500 cm, resolution ratio was 1 cm, air was regarded as blank, the scanning number was 16, amplification was one time;MOA, MOB and linoleic acid levels of MaiDong extracting solution were measured by using HPLC, Grace Alltima C18 (4.6 mm ×250 mm, 5 μm) was adopted as chromatographic column, acetonitrile as moving phase B, gradient elution was using moving phase A of 1mmol/L ammonium acetate aqueous solution, flow rate was 1.0 mL/min, column temperature was 30℃, detection wavelength was 207nm, super area-external standard method was used. The detection results were compared and studied. Results:Three components of MaiDong extracting solution nearly reached to balance within two hours during two processes of extraction, level changes of three components in MaiDong from different batches extracting solution were nearly similar, and there was no significant difference between them. Conclusion:Online near-infrared spectrum technology is verified by methodology, which can be used for monitoring extraction technology of MaiDong.