摘要: |
[摘要]目的:采用高效液相一测多评(HPLC-QAMS)法,建立小儿清热化痰栓中马钱子苷、当药苷、断氧化马钱子苷、甘草苷、甘草酸、连翘酯苷B、连翘酯苷A和连翘苷含量的检测方法。方法:采用Agilent Zorbax SB-C18色谱柱,以乙腈-0.2%磷酸水溶液为流动相,梯度洗脱;检测波长分别为237 nm(检测马钱子苷、当药苷、断氧化马钱子苷、甘草苷和甘草酸)和275 nm(检测连翘酯苷B、连翘酯苷A和连翘苷);流速1.0 mL/min;柱温30 ℃。以甘草苷为内参物,通过测定其与马钱子苷、当药苷、断氧化马钱子苷、甘草酸、连翘酯苷B、连翘酯苷A和连翘苷的相对校正因子(RCF),计算各成分含量,同时与外标法(ESM)实测值进行对比,验证HPLC-QAMS的可行性。结果:马钱子苷、当药苷、断氧化马钱子苷、甘草苷、甘草酸、连翘酯苷B、连翘酯苷A和连翘苷质量浓度分别在4.08~102.00、0.77~19.25、4.59~114.75、1.35~33.75、2.74~68.50、1.61~40.25、7.73~193.25、2.19~54.75 μg/mL范围内与峰面积线性关系良好(r≥0.999 1),平均加样回收率及RSD分别为99.45%(0.96%)、97.49%(1.45%)、98.85%(1.08%)、99.13%(0.78%)、100.04%(0.76%)、98.63%(1.59%)、100.07%(0.60%)和96.99%(1.26%)。小儿清热化痰栓中各成分HPLC-QAMS计算含量值与外标法实测含量值无明显差异。结论:所建立的HPLC-QAMS操作简便易行,成本较低,可用于小儿清热化痰栓多指标成分的质量评价。 |
关键词: 小儿清热化痰栓 高效液相一测多评法 多指标成分 相对校正因子 质量评价 |
DOI:doi:10.13407/j.cnki.jpp.1672-108X.2022.10.008 |
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基金项目: |
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Determination of 8 Main Components in Xiao’er Qingre Huatan Suppository by High Performance Liquid Chromatography-Quantitative Analysis of Multi-Components by Single-Marker |
Zhang Chuanxiang1, He Miao1, Ma Danfeng1, Wang Haibin2 |
(1. Hunan Children’s Hospital, Changsha 410007, China; 2. Hunan Institute for Drug Control, Changsha 410001, China) |
Abstract: |
[Abstract] Objective: To establish the determination method of loganin, sweroside, secoxyloganin, liquiritin, glycyrrhizic acid, forsythoside B, forsythoside A and forsythin in Xiao’er Qingre Huatan suppository based on high performance liquid chromatography-quantitative analysis of multi-components by single-marker (HPLC-QAMS) method. Methods: Agilent Zorbax SB-C18 was adopted, acetonitrile-0.2% phosphoric acid solution was the mobile phase by gradient elution. The detection wavelength was set at 237 nm for loganin, sweroside, secoxyloganin, liquiritin and glycyrrhizic acid, and 275 nm for forsythoside B, forsythoside A and forsythin. The flow rate was 1.0 mL/min at column temperature of 30 ℃. Liquiritin was used as an internal standard, the relative correction factors (RCF) of loganin, sweroside, secoxyloganin, glycyrrhizic acid, forsythoside B, forsythoside A and forsythin were calculated. The method was validated by comparison of the quantitative results between external standard method (ESM) and HPLC-QAMS method. Results: Loganin, sweroside, secoxyloganin, liquiritin, glycyrrhizic acid, forsythoside B, forsythoside A and forsythin showed good linear relationships within the ranges from 4.08 to 102.00, from 0.77 to 19.25, from 4.59 to 114.75, from 1.35 to 33.75, from 2.74 to 68.50, from 1.61 to 40.25, from 7.73 to 193.25 and from 2.19 to 54.75 μg/mL (r≥0.999,1), the average recoveries and RSD were respectively 99.45% (0.96%), 97.49% (1.45%), 98.85% (1.08%), 99.13% (0.78%), 100.04% (0.76%), 98.63% (1.59%), 100.07% (0.60%) and 96.99% (1.26%). There was no significant difference between the contents calculated by HPLC-QAMS and measured by external standard method for each component in Xiao’er Qingre Huatan suppository. Conclusion: The HPLC-QAMS method is simple with lower cost, and can be used for the multi-index component quality evaluation of Xiao’er Qingre Huatan suppository. |
Key words: Xiao’er Qingre Huatan suppository high performance liquid chromatography-quantitative analysis of multi-components by single-marker multi-index components relative correction factor quality evaluation |