| 乔莉,简淑仪,赖竹仪,李华,黄俊忠.超高效液相色谱法检测小柴胡颗粒中掺入的黄芩提取物[J].中国药事,2023,(4):450-460 |
| 超高效液相色谱法检测小柴胡颗粒中掺入的黄芩提取物 |
| Determination of Scutellaria Extract Added in Xiaochaihu Granules by UPLC |
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| DOI：10.16153/j.1002-7777.2023.04.012 |
| 中文关键词: 黄芩提取物 汉黄芩苷 黄芩苷 小柴胡颗粒 掺入 超高效液相色谱 |
| 英文关键词: Scutellaria extract wogonoside baicalin Xiaochaihu granules added UPLC |
| 基金项目: |
| 作者 | 单位 | | 乔莉 | 广东省药品检验所,国家药品监督管理局药品快 速检验技术重点实验室,广东省药品监督管理局粤港澳大湾区中药标准研究重点实验室,广州 510663 | | 简淑仪 | 广东省药品检验所,国家药品监督管理局药品快 速检验技术重点实验室,广东省药品监督管理局粤港澳大湾区中药标准研究重点实验室,广州 510663 | | 赖竹仪 | 广东省药品检验所,国家药品监督管理局药品快 速检验技术重点实验室,广东省药品监督管理局粤港澳大湾区中药标准研究重点实验室,广州 510663 | | 李华 | 广东省药品检验所,国家药品监督管理局药品快 速检验技术重点实验室,广东省药品监督管理局粤港澳大湾区中药标准研究重点实验室,广州 510663 | | 黄俊忠 | 广东省药品检验所,国家药品监督管理局药品快 速检验技术重点实验室,广东省药品监督管理局粤港澳大湾区中药标准研究重点实验室,广州 510663 |
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| 中文摘要: |
| 目的：建立小柴胡颗粒中掺入黄芩提取物的检测方法。方法：采用超高效液相色谱法，以汉黄芩苷与黄芩苷峰面积的比值作为指标对小柴胡颗粒中是否掺入黄芩提取物进行分析。采用Waters CORTECS® T3(100 mm ×4.6 mm，2.7 μm)色谱柱；以甲醇(A)-0.5%甲酸(B)为流动相，梯度洗脱(0~10 min，5%A→25%A；10~40 min，25%A→55%A；40~55 min，55%A→80%A)；流速 0.6 mL·min-1；检测波长 270 nm；柱温 30 ℃；进样量 5 μL。结果：精密度、重复性、稳定性试验的RSD 分别为0.032%(n=6)、0.011%和2.3%(n=6)、0.094%(n=8)，掺入黄芩提取物的比例在0%~100% 与汉黄芩苷和黄芩苷峰面积比值线性关系良好(r=0.993)。对199批次小柴胡颗粒样品进行检测，结果检出阳性样品(峰面积比值＜0.10)48批次。结论：该方法简单快速、准确可靠，专属性强，耐用性良好，可用于检测小柴胡颗粒中掺入黄芩提取物，为监管提供技术支撑。 |
| 英文摘要: |
| Objective: To establish a method for the detection of Scutellaria Extract added in Xiaochaihu granules. Methods: The peak areas ratio of baicalin and wogonoside was used as an index to analyze whether Xiaochaihu granules were added with Scutellaria extract by UPLC. The separation was performed on Waters CORTECS® T3 (100 mm ×4.6 mm, 2.7 µm) column, the mobile phase was composed of methanol (A) and 0.5% formic acid (B) with gradient elution (0-10 min, 5% A→25% A; 10-40 min, 25% A→55% A; 40-55 min, 55% A→80% A), the fl ow rate was 0.6 mL·min-1, the detection wavelength was 270 nm, the column temperature was 30 ℃ and the injection volume was 5 µL. Results: RSD of precision, repeatability and stability test were 0.032%(n=6), 0.011% and 2.3% (n=6), 0.094% (n=8), respectively. There was a good linear relationship between the proportion of added with Scutellaria extract at 0%-100% and the peak area ratio of baicalin and wogonoside (r=0.993). The established method was used to analyze 199 batches of Xiaochaihu granules, and 48 positive samples (Peak area ratio＜0.10) were detected of them. Conclusion: This method is simple, rapid, accurate and reliable, and could be used to detect the illegal mixed of Scutellaria extract in Xiaochaihu granules, which provides technical support for supervision. |
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