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目的:建立漂浮有机液滴凝固液相微萃取-高效液相色谱(SFOD-LPME-HPLC)法测定金线莲中对羟基苯乙酮和香草乙酮含量的方法。方法:利用SFOD-LPME技术对中药材金线莲中低峰度组分对羟基苯乙酮和香草乙酮进行富集,最后运用HPLC进行分析。优化后的萃取实验条件:60μL的十二醇为萃取溶剂,1 000μL的四氢呋喃为分散溶剂,15 mL样液加入氯化钠4.50 g,pH为4.0,40℃水浴,以1 500 r·min~(-1)转速搅拌萃取40 min。色谱条件:色谱柱:Agilent TC-C18(4.6 mm×250mm,5μm);流动相:甲醇-0.1%乙酸(25∶75);流速:1.0mL·min~(-1);柱温:31.5℃;检测波长:275 nm。结果:对羟基苯乙酮和香草乙酮的线性范围均为2~24 ng·mL~(-1),检测限分别为0.06 ng·mL~(-1)和0.17 ng·mL~(-1),富集倍数分别为166和140,测得福建南靖组培金线莲中对羟基苯乙酮和香草乙酮的含量分别为1.69μg·g~(-1)和0.72μg·g~(-1),回收率在95.29%~104.30%之间。结论:该法具有集富集、净化于一体的特点,可成为简单、可靠、快速的中药质量控制前处理和测定方法。
OBJECTIVE: To establish a method for the determination of p-hydroxyacetophenone and vanillin in Anoectochilus roxburghii by SFOD-HPLC with floating organic liquid. Methods: SFOD-LPME was used to enrich the mid and low peak components of Chinese herbal medicine, Hydroxyacetophenone and Vanillin, and finally analyzed by HPLC. Optimized extraction conditions: 60μL of dodecanol as extraction solvent, 1000μL of tetrahydrofuran as the dispersion solvent, 15mL sample solution was added sodium chloride 4.50g, pH 4.0, 40 ℃ water bath, with 1 500 r · min ~ (-1) speed stirring extraction 40 min. Chromatographic conditions: column: Agilent TC-C18 (4.6 mm × 250 mm, 5 μm); mobile phase: methanol -0.1% acetic acid (25:75); flow rate: 1.0 mL · min -1; Detection wavelength: 275 nm. Results: The linear range of p - hydroxyacetophenone and vanillin was 2 ~ 24 ng · mL -1 with the detection limits of 0.06 ng · mL -1 and 0.17 ng · mL -1, respectively ) And the enrichment multiple were 166 and 140, respectively. The contents of p-hydroxyacetophenone and vanillin in the tissue culture of Nanning, Fujian were 1.69μg · g ~ (-1) and 0.72μg · g ~ (-1). The recoveries ranged from 95.29% to 104.30%. Conclusion: The method has the characteristics of enrichment and purification and can be a simple, reliable and rapid pretreatment and determination method for quality control of traditional Chinese medicine.