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目的:建立测定蒜氨酸含量和有关物质的高效离子交换色谱法。方法:采用Hypersil SCX柱(250mm×4.6mm,5μm,氢型阳离子交换色谱柱),以磷酸盐缓冲液(取磷酸二氢钾13.6g,加水溶解并稀释成1000mL,用85%磷酸调pH至2.0)为流动相,流速1.0mL·min-1,检测波长214nm,柱温30℃,进样量20μL。结果:蒜氨酸及其有关物质色谱分离良好,蒜氨酸浓度在0.06～1.8mg·mL-1的范围内线性关系良好(r=0.9999),平均加样回收率(n=9)为100.2%,精密度良好(日内RSD=1.2%,n=5;日间RSD=1.4%,n=5),检测限(S/N=3)为0.16μg·mL-1。结论:本方法准确、快速,重复性好,可用于蒜氨酸含量和有关物质测定,适合蒜氨酸制备过程的质量控制。
Objective: To establish a high performance ion exchange chromatography method for the determination of alliin content and related substances. Methods: Hypersil SCX column (250mm × 4.6mm, 5μm, hydrogen type cation exchange column) was used as a phosphate buffer solution (13.6g of potassium dihydrogen phosphate, dissolved in water and diluted to 1000mL, pH was adjusted to 85% phosphoric acid 2.0) for the mobile phase, flow rate 1.0mL · min-1, detection wavelength 214nm, column temperature 30 °C, injection volume 20μL. RESULTS: The chromatographic separation of alliin and its related substances was good. The linear relationship between the concentration of alliin in the range of 0.06-1.8 mg·mL-1 was good (r=0.9999) and the average recovery (n=9) was 100.2. %, with good precision (dayday RSD = 1.2%, n = 5; daytime RSD = 1.4%, n = 5), and the detection limit (S/N = 3) was 0.16 μg·mL-1. Conclusion: The method is accurate, rapid, and reproducible. It can be used for the determination of alliin and related substances, and is suitable for the quality control of the preparation of alliin.