首页|蓝芩颗粒高效液相色谱指纹图谱的建立及9个指标成分含量测定

蓝芩颗粒高效液相色谱指纹图谱的建立及9个指标成分含量测定

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目的 建立蓝芩颗粒的高效液相色谱(HPLC)指纹图谱,并测定其中指标成分含量。方法 色谱柱为 Agilent Infinity Lab Poroshell 120 EC-C18 柱(150 mm×4。6 mm,2。7µm),流动相为乙腈-0。02mol/L磷酸二氢钠溶液(pH 4。2)、梯度洗脱,流速为1。0 mL/min,检测波长为 230 nm,柱温为 30℃,进样量为 10µL。采用中药色谱指纹图谱相似度评价系统(2012 版)绘制 12 批样品的特征图谱,计算相似度;确定共有峰并指认,并同时测定指认出的成分含量。结果 蓝芩颗粒HPLC指纹图谱中有 23 个共有峰,相似度均大于 0。92。指认出其中 9 个,分别为(R,S)-告依春、京尼平龙胆双糖苷、栀子苷、盐酸黄柏碱、黄芩苷、千层纸素A-7-O-β-D-葡萄糖醛酸苷、汉黄芩苷、盐酸小檗碱、汉黄芩素,其质量浓度分别在 0。026 2~7。815µg/mL、0。204 0~411。600µg/mL、0。122 2~377。400µg/mL、0。195 1~15。360µg/mL、0。078 7~297。000µg/mL、0。092 0~410。103µg/mL、0。201 9~149。625µg/mL、0。101 8~7。538µg/mL、0。101 9~19。200µg/mL范围内与峰面积线性关系良好(r≥0。999 8);检测限为 0。006 5~0。051 1µg/mL,定量限为 0。026 2~0。204 0µg/mL;中间精密度、稳定性、重复性试验结果的 RSD均小于 3。0%,平均加样回收率为 96。37%~101。69%,RSD为 0。48%~0。91%(n=6)。结论 该方法灵敏、简便、准确,可用于蓝芩颗粒的质量控制。
Establishment of HPLC Fingerprint of Lanqin Granules and Content Determination of Nine Indicator Components
Objective To establish a high-performance liquid chromatography(HPLC)fingerprint of Lanqin Granules,and to determine the contents of nine indicator components.Methods The chromatographic column was the Agilent Infinity Lab Poroshell 120 EC-C18 column(150 mm×4.6 mm,2.7 µm),the mobile phase was acetonitrile-0.02 mol/L sodium dihydrogen phosphate solution(pH 4.2)with gradient elution,the flow rate was 1.0 mL/min,the detection wavelength was 230 nm,the column temperature was 30℃,and the injection volume was 10 µL.The characteristic HPLC fingerprint of 12 batches of samples was established by the Similarity Evaluation System for Chromatographic Fingerprint of Traditional Chinese Medicine(2012 Version),and the similarity was calculated;the common peaks were marked and identified,and the contents of identified components were determined.Results There were 23 common peaks in the HPLC fingerprint of Lanqin Granules,with a similarity greater than 0.92.Nine of them were identified,including(R,S)-goitrin,genipin 1-gentiobioside,geniposide,phellodendrine chloride,baicalin,oroxyloside,wogonoside,berberine hydrochloride,wogonin.The contents of the above nine components were 0.026 2-7.815 µg/mL,0.204 0-411.600 µg/mL,0.122 2-377.400 µg/mL,0.195 1-15.360 µg/mL,0.078 7-297.000 µg/mL,0.092 0-410.103 µg/mL,0.201 9-149.625 µg/mL,0.101 8-7.538 µg/mL,0.101 9-19.200 µg/mL(r≥0.999 8),respectively.The limits of detection(LOD)were in the range of 0.006 5-0.051 1 µg/mL,and the limits of quantification(LOQ)were in the range of 0.026 2-0.204 0 µg/mL.The RSDs of the intermediate precision,stability and repeatability tests were all lower than 3.0%.The average recovery rates of the above nine components were in the range of 96.37%-101.69%,with the RSDs in the range of 0.48%-0.91%(n=6).Conclusion This method is sensitive,simple,and accurate,which can be used for the quality control of Lanqin Granules.

Lanqin GranulesHPLCfingerprintcontent determination

潘燕、胡林水、许超、吴晓琼、王成芳

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浙江康恩贝制药股份有限公司,浙江 金华 321109

浙江省中药制药技术重点实验室,浙江 金华 321109

蓝芩颗粒 高效液相色谱法 指纹图谱 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(18)