SFOD-LPME-HPLC测定金线莲中对羟基苯乙酮和香草乙酮

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：60 μL的十二醇为萃取溶剂，1 000 μL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×250 mm，5 μm）；流动相：甲醇-0.1%乙酸（25：75）；流速：1.0 mL·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1.69 μg·g^-1和0.72 μg·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。

Determination of 4-acetylphenol and apocynin in Anoectochilus roxburghii by SFOD-LPME-HPLC

OBJECTIVE To establish a method for determination of 4-acetylphenol and apocynin in Anoectochilus roxburghii by high performance liquid chromatography (HPLC)-liquid phase microextraction method based on solidification of floating organic drop microextraction (SFOD-LPME). METHODS 4-acetylphenol and apocynin in Anoectochilus roxburghii were determined by HPLC method after enrichment prior of SFOD-LPME. The optional microextraction experiment conditions were as follows:60 μL of dodecanol as extraction solvent, 1 000 μL of tetrahydrofuran as dispersive solvent, 4.5 g NaCl added in 15 mL sample volume, pH of the sample 4.0, the sample was extracted in 40℃ water bath and centrifuged at 1 500 r·min^-1 for 40 minutes. Quantitative analysis was carried out on a Agilent TC-C₁₈ (4.6 mm×250 mm, 5 μm) by simultaneous HPLC, using a mobile phase of methanol-0.1% acetic acid (25:75) at a flow rate of 1.0 mL·min^-1 at 31.5℃. Detection wavelength was set at 275 nm. RESULTS 4-acetylphenol and apocynin both had good linear relationship in range of 2-24 ng·mL^-1 and detection limits were 0.06 ng·mL^-1 and 0.17 ng·mL^-1, respectively, with enrichment factors of 166 and 140. The contents of 4-acetylphenol and apocynin in Anoectochilus roxburghii were 1.69 μg·g^-1 and 0.72 μg·g^-1, respectively. The recovery range was 95.29%-104.30%. CONCLUSION The method in this paper both has advantages of preconcentration and purification and can be used as a simple, accurate and fast method for quality control of traditional Chinese medicine in pre-treatment and determination.