高效液相色谱-内标法测定焦性没食子酸含量

摘要

A rapid, specific, and accurate HPLC method was developed and validated for the assay of pyrogallol. The assay involved a gradient elution of pyrogallol with a Thermo Hypersil C18 column (250 mm × 4. 6 mm,5 μm) using mobile phase composition of methanol and water (0. 1% TFA) at a flow rate of 1. 0 mL/min. UV detection was performed at 266 nm. Ellagic acid was used as an internal standard. The retention time of pyrogallol and ellagic acid was 4. 33 and 19. 25 min,respectively. The linearity range of pyrogallol concentration was from 62. 5 to 2 000 mg/L. The fitting equation of calibration curve was y =0. 000 138 66x+0. 001 92 (R=0. 999 7) and a mean recovery of 103. 6% was found. The proposed method was applied for the quantitative determination of pyrogallol in pyrogallol products.%建立了一种方便、快速、准确的测定焦性没食子酸含量的高效液相色谱-内标分析方法。色谱条件为：Thermo HypersilC18(250mm×4.6mm,5μm)色谱柱,流动相为甲醇/水(含0.1%的三氟乙酸),梯度洗脱,流速为1.0mL/min,紫外检测波长为266 nm。选择鞣花酸作为内标物。结果表明在该色谱条件下,焦性没食子酸和鞣花酸的保留时间分别为4.33和19.25 min,焦性没食子酸质量浓度在62.5~2000 mg/L范围内呈良好线性关系,线性方程y=0.00013866x+0.00192(R=0.9997),平均加样回收率为103.6%。该方法简便、准确、重现性好,可适用于焦性没食子酸产品含量的分析测定。