HPLC-CAD法同时测定风湿定片中7种活性成分的含量
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篇名: | HPLC-CAD法同时测定风湿定片中7种活性成分的含量 |
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摘要: | 目的:建立同时测定风湿定片中甘草酸、水杨苷、甘草次酸、毒藜碱、丹皮酚、欧前胡素及异欧前胡素含量的方法。方法:采用高效液相色谱-电雾式检测器(HPLC-CAD)法。色谱柱为Thermo Hypersil BDS C18,流动相为乙腈-10 mmol/L甲酸铵(甲酸调pH至4.5,梯度洗脱),流速为1.0 mL/min,柱温为35 ℃,CAD雾化器温度为35 ℃,气压为(59.6±0.1) psi,检测频率为10 Hz,进样量为20 μL。结果:甘草酸、水杨苷、甘草次酸、毒藜碱、丹皮酚、欧前胡素及异欧前胡素检测质量浓度线性范围为0.42~16.80、0.28~11.20、0.16~6.20、0.98~39.40、1.02~41.00、0.11~4.40、0.10~3.80 μg/mL(r≥0.999 1);检测限分别为0.03、0.02、0.02、0.03、0.03、0.02、0.02 μg/mL,定量限分别为0.11、0.06、0.06、0.10、0.11、0.08、0.07 μg/mL;精密度、稳定性(48 h)、重复性试验的RSD均<2.0%(n=6或n=7);平均回收率为98.61%~99.76%,RSD为1.11%~1.51%(n=6)。结论:建立的方法操作简便、灵敏度高、结果准确,可用于风湿定片中甘草酸、水杨苷、甘草次酸、毒藜碱、丹皮酚、欧前胡素及异欧前胡素含量的同时测定。 |
ABSTRACT: | OBJECTIVE: To establish the method for simultaneous determination of glycyrrhizic acid, salicin, glycyrrhetinic acid, chenopodium, paeonol, imperatorin and isoimperatorin in Fengshiding tablet. METHODS: HPLC-CAD method was adopted. The determination was performed on Thermo Hypersil BDS C18 column with mobile phase consisted of acetonitrile-10 mmol/L ammonium formate (pH value adjusted to 4.5 using formic acid, gradient elution) at the flow rate of 1.0 mL/min. The column temperature was set at 35 ℃. CAD atomizer temperature was 35 ℃, and air pressure was (59.6±0.1) psi. The detection frequency was 10 Hz, and sample size was 20 μL. RESULTS: The linear range of glycyrrhizic acid, salicin, glycyrrhetinic acid, chenopodium, paeonol, imperatorin and isoimperatorin were 0.42-16.80, 0.28-11.20, 0.16-6.20, 0.98-39.40, 1.02-41.00, 0.11- 4.40, 0.10-3.80 μg/mL(r≥0.999 1), respectively. The detection limits were 0.03, 0.02, 0.02, 0.03, 0.03, 0.02, 0.02 μg/mL, respectively; quantitation limits were 0.11, 0.06, 0.06, 0.10, 0.11, 0.08, 0.07μg/mL, respectively. RSDs of precision, stability (48 h) and reproducibility tests were all lower than 2.0% (n=6 or n=7). Average recoveries rate were 98.61%-99.76%, and RSDs were 1.11%-1.51% (n=6). CONCLUSIONS: The established method is simple, sensitive, accurate, and can be used for simultaneous determination of glycyrrhizic acid, salicin, glycyrrhetinic acid, chenopodium, paeonol, imperatorin and isoimperatorin in Fengshiding tablet. |
期刊: | 2018年第29卷第23期 |
作者: | 侯爱荣,邢晔忠,吴雪松 |
AUTHORS: | HOU Airong,XING Yezhong,WU Xuesong |
关键字: | 高效液相色谱-电雾式检测器法;风湿定片;水杨苷;毒藜碱;丹皮酚;欧前胡素;含量测定 |
KEYWORDS: | HPLC-CAD; Fengshiding tablet; Salicin; Chenopodium; Paeonol; Imperatorin; Content determination |
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