波长转换RP-HPLC法同时测定茯苓不同部位中5种三萜酸含量

车  爽  李  清  霍艳双  陈晓辉  毕开顺

波长转换RP-HPLC法同时测定茯苓不同部位中5种三萜酸含量

车爽李清霍艳双陈晓辉毕开顺

RP-HPLC simultaneous determination of five triterpenoid acids in different parts of Poria cocos by UV wavelengths switch

CHE Shuang

摘要

摘要:
建立同时测定茯苓不同部位中去氢土莫酸、猪苓酸C、3-表去氢土莫酸、去氢茯苓酸和茯苓酸含量的方法。采用紫外-波长转换检测的RP-HPLC法: 色谱柱为Kromasil C₁₈柱 (250 mm × 4.6 mm, 5 μm); 流动相为乙腈 (A)-0.05%磷酸水溶液 (B) 系统, 梯度洗脱 (0～5 min, 60%A～64%A; 5～35 min, 64%A～65%A; 35～35.01 min, 65% A～73% A; 35.01～53 min, 73% A); 流速为1.0 mL·min⁻¹; 检测波长为0～48 min, 241 nm (去氢土莫酸、猪苓酸C、3-表去氢土莫酸、去氢茯苓酸), 48～55 min, 210 nm (茯苓酸)。去氢土莫酸、猪苓酸C、3-表去氢土莫酸、去氢茯苓酸和茯苓酸分别在30.5～610.0 μg·mL⁻¹ (r = 0.999 6)、12.66～253.2 μg·mL⁻¹ (r = 0.999 5)、2.99～59.7 μg·mL⁻¹ (r = 0.999 7)、6.13～122.5 μg·mL⁻¹ (r = 0.999 5)、11.3～226.0 μg·mL⁻¹ (r = 0.999 5) 内浓度与峰面积呈良好的线性关系; 方法回收率分别为98.5% (RSD = 1.9%)、99.4% (RSD = 1.7%)、97.9% (RSD = 1.2%)、96.7% (RSD = 2.5%) 和97.9% (RSD = 2.3%)。结果表明, 本方法简便、准确、重现性好, 为茯苓药材的质量控制提供了依据。

Abstract:
To establish a method for simultaneous determination of dehydrotumulosic acid, polyporenic acid C, 3-epi-dehydrotumulosic acid, dehydropachymic acid and pachymic acid in Poria, a RP-HPLC method detected by UV wavelengths switch had been developed, including 210 nm (48−55 min) for pachymic acid and 241 nm (0−48 min) for dehydrotumulosic acid, polyporenic acid C, 3-epi-dehydrotumulosic acid, dehydropachymic acid, separately. The system consisting of a Kromasil C₁₈ column (250 mm × 4.6 mm, 5 μm) and a mixture of acetonitrile and 0.05% phosphate acid as the mobile phase was adopted; The flow rate was 1.0 mL·min⁻¹. The linear response range was 30.5−610.0 μg·mL⁻¹ (r = 0.999 6) for dehydrotumulosic acid, 12.66−253.2 μg·mL⁻¹ (r = 0.999 5) for polyporenic acid C, 2.99−59.7 μg·mL⁻¹ (r = 0.999 7) for 3-epi-dehydrotumulosic acid, 6.13−122.5 μg·mL⁻¹ (r = 0.999 5) for dehydropachymic acid and 11.3−226.0 μg·mL⁻¹ (r = 0.999 5) for pachymic acid. The average recoveries of these compounds were 98.5% (RSD = 1.9%), 99.4% (RSD = 1.7%), 97.9% (RSD = 1.2%), 96.7% (RSD = 2.5%) and 97.9% (RSD = 2.3%), respectively. The method is simple, accurate and reproducible for quality control of Poria.

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