| 王春燕,郭鑫,陈艳梅,等.固相萃取 -高效液相色谱法测定妇乐颗粒中大黄素、大黄酸、绿原酸和没食子酸的含量[J].安徽医药,2023,27(5):907-910. |
| 固相萃取 -高效液相色谱法测定妇乐颗粒中大黄素、大黄酸、绿原酸和没食子酸的含量 |
| Determination of emodin, rhubarb acid, chlorogenic acid and gallic acid in fule granules by solid phase extraction purification combined with HPLC |
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| DOI：10.3969/j.issn.1009-6469.2023.05.012 |
| 中文关键词: 主成分分析 固相萃取 高效液相色谱 妇乐颗粒 |
| 英文关键词: Principal component analysis Solid phase extraction High performance liquid chromatography Fule granules |
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| 中文摘要: |
| 目的建立了固相萃取 -高效液相色谱法测定妇乐颗粒中大黄素、大黄酸、绿原酸和没食子酸的含量，从洗脱溶剂的种类与体积、流动相的组成等条件优化检测方法。方法采用 HLB萃取小柱净化， 3 mL的乙腈 -乙酸(95∶5)作为洗脱溶剂； Ther-mo C18柱( 150 mm×4.6 mm，5 μm)进行分离，流动相为质量分数为 0.1%磷酸水溶液( A)-乙腈( B)梯度洗脱，洗脱程序如下: 0～ 1 min，30% B；1～3 min，70% B；3～6 min，70% B；6～8 min，30% B；流速为 1.0 mL/min，检测波长为 254 nm(大黄酸和大黄素)、 270 nm(没食子酸)、 325 nm(绿原酸)，柱温为 25 ℃，进样量为 20 μL。结果在最优的萃取条件下所建立的方法定量限为 5～20 mg/L，日内、日间精密度均小于 5.2%，加样回收率为 95.07%～98.74%，RSD值小于 5.3%。结论该方法准确、灵敏和重复性好，为完善妇乐颗粒质量控制体系提供理论基础和实用依据。 |
| 英文摘要: |
| Objective To establish a solid phase extraction method-high performance liquid chromatographic analysis for the deter-mination of emodin, rhein, gallic acid and chlorogenic acid from fule granules samples, and to optimize the detection method from thetypes and volumes of elution solvents and the composition of mobile phases.Methods The HLB extraction cartridge was used for puri-fication with 3 mL of acetonitrile acetic acid (95∶5) as elution solution. The Thermo C18 column (150 mm×4.6 mm, 5 μm) was used toseparation. The mobile phase was gradient elution of 0.1% phosphoric acid solution (A)/acetonitrile (B). The elution procedure was asfollows: 0-1 min, 30% B; 1-3 min, 70% B; 3-6 min, 70% B; 6-8 min, 30% B. The flow rate was 1.0 mL/min, the detection wavelengthswere set at 254 nm (emodin and rhein), 270 nm (gallic acid) and 325 nm (chlorogenic acid). Column temperature was 25 ℃ with 20 μLof injection volume.Results Under the optimal extraction condition, the quantitative limit of the method was 5-20 mg/L, and the intra-day and interday precision was less than 5.2%, the recovery rate was 95.07%-98.74% with RSD<5.3%.Conclution The developedmethod is accurate, sensitive and reproducible, which provides theoretical basis and practical introduction for improving the qualitycontrol system of fule granules. |
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