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高效液相色谱法同时测定启脾丸中9种成分含量

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目的 建立同时测定启脾丸中 9 种成分含量的高效液相色谱-二极管阵列检测器(HPLC-DAD)法。方法 色谱柱为Agilent Extend C18 柱(250 mm×4。6 mm,5µm),流动相为甲醇-乙腈(1∶1,V/V)-0。08%磷酸水溶液(梯度洗脱),流速为 1。0 mL/min,检测波长分别为 237 nm(甘草苷、甘草酸铵)、283 nm(橙皮苷)、203 nm(人参皂苷Rg1、人参皂苷Re)、220 nm(白术内酯Ⅲ、白术内酯Ⅱ、白术内酯Ⅰ、茯苓酸),柱温为 30℃,进样量为 10µL。结果 甘草苷、甘草酸铵、橙皮苷、人参皂苷Rg1、人参皂苷Re、白术内酯Ⅲ、白术内酯Ⅱ、白术内酯Ⅰ、茯苓酸的质量浓度分别在3。66~58。48µg/mL、6。21~99。41µg/mL、9。53~152。54µg/mL、3。06~48。89µg/mL、1。51~24。11µg/mL、2。54~40。60µg/mL、1。24~19。78µg/mL、2。10~33。64µg/mL、3。57~57。08µg/mL范围内与峰面积线性关系良好(r≥0。9995,n=6);精密度、重复性、稳定性试验结果的RSD均小于 2。0%(n=6);平均加样回收率分别为 100。34%,101。35%,101。18%,99。65%,98。73%,98。86%,100。86%,99。30%,100。86%,RSD分别为 1。43%,1。52%,0。68%,1。43%,1。00%,1。19%,1。31%,0。75%,1。36%(n=6)。样品中 9 种成分的含量分别为 0。526 4~1。100 7 mg/g、0。956 2~1。700 2 mg/g、1。125 2~1。876 2 mg/g、0。5709~0。8256 mg/g、0。1014~0。5026 mg/g、0。2269~0。6117 mg/g、0。0994~0。3705 mg/g、0。1525~0。4164 mg/g、0。395 2~0。755 6 mg/g(n=3)。结论 该方法操作简便、专属性强、稳定性好、结果准确,可用于启脾丸中 9 种成分含量的同时测定。
Simultaneous Determination of Nine Components in Qipi Pills by HPLC
Objective To establish a high-performance liquid chromatography-diode array detector(HPLC-DAD)method for simultaneous determination of nine components in Qipi Pills.Methods The chromatographic column was Agilent Extend C18 column(250 mm×4.6 mm,5 µm),the mobile phase was methanol acetonitrile(1∶1,V/V)-0.08%phosphoric acid aqueous solution(gradient elution),the flow rate was 1.0 mL/min,the detection wavelength was set at 237 nm for liquiritin and ammonium glycyrrhizinate,283 nm for hesperidin,203 nm for ginsenoside Rg1 and ginsenoside Re,220 nm for atracylenolide Ⅲ,atracylenolide Ⅱ,atracylenolide Ⅰ,and pachymic acid,the column temperature was 30℃,and the injection volume was 10 µL.Result The linear ranges of liquiritin,ammonium glycyrrhizinate,hesperidin,ginsenoside Rg1,ginsenoside Re,atracylenolide Ⅲ,atracylenolide Ⅱ,atracylenolide Ⅰ and pachymic acid were 3.66-58.48 µg/mL,6.21-99.41 µg/mL,9.53-152.54 µg/mL,3.06-48.89 µg/mL,1.51-24.11 µg/mL,2.54-40.60 µg/mL,1.24-19.78 µg/mL,2.10-33.64 µg/mL,and 3.57-57.08 µg/mL(r≥0.999 5,n=6).The RSDs of precision,repeatability,and stability test results were all lower than 2.0%(n=6).The average recoveries of the above nine components were 100.34%,101.35%,101.18%,99.65%,98.73%,98.86%,100.86%,99.30%and 100.86%,with RSDs of 1.43%,1.52%,0.68%,1.43%,1.00%,1.19%,1.31%,0.75%,and 1.36%(n=6),respectively.The contents of the above nine components in samples were in the ranges of 0.526 4-1.100 7 mg/g,0.956 2-1.700 2 mg/g,1.125 2-1.876 2 mg/g,0.570 9-0.825 6 mg/g,0.101 4-0.502 6 mg/g,0.226 9-0.611 7 mg/g,0.099 4-0.370 5 mg/g,0.152 5-0.416 4 mg/g,and 0.395 2-0.755 6 mg/g(n=3),respectively.Conclusion The method is simple,has strong specificity,good stability,and accurate results,which can be used for the simultaneous determination of nine components in Qipi Pills.

HPLCDADQipi Pillscontent determination

米振清、胡小凤

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山东省泰安市食品药品检验检测研究院·山东省泰安市纤维检验所,山东 泰安 271000

山东鲁抗医药集团赛特有限责任公司,山东 泰安 271200

高效液相色谱法 二极管阵列检测器 启脾丸 含量测定

2024

中国药业
重庆市食品药品监督管理局

中国药业

CSTPCD
影响因子:1.369
ISSN:1006-4931
年,卷(期):2024.33(11)
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