基于指纹图谱结合化学计量学及多成分含量测定的壁钱质量研究

doi:10.11669/cpj.2022.22.010

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摘要目的建立壁钱的HPLC指纹图谱和多指标成分的含量测定方法,并结合化学计量学方法评价其质量。方法采用Waters Symmetry RP C₁₈色谱柱,以甲醇(A)-体积分数0.1% 冰醋酸溶液(B)为流动相,梯度洗脱(0～15 min,0 A;15～18 min,0~10% A;18～30 min,10%~15% A),检测波长为262 nm,流速:0.5 mL·min^-1,柱温:35 ℃。对壁钱药材、饮片和焙壁钱进行指纹图谱构建,并结合相似度分析和化学计量学分析,同时测定尿嘧啶、鸟嘌呤、次黄嘌呤、尿苷、肌苷和鸟苷的含量。结果 30批壁钱样品指纹图谱相似度均在0.96以上,共标定了17个共有峰,指认出6个色谱峰,分别是尿嘧啶、鸟嘌呤、次黄嘌呤、尿苷、肌苷和鸟苷。聚类分析将30批壁钱样品分为3类,不同炮制规格各自聚为一类。主成分分析表明,不同药材市场的壁钱样品间存在差异,不同炮制方式壁钱样品间差异较小。尿嘧啶、鸟嘌呤、次黄嘌呤、尿苷、肌苷及鸟苷的质量分数范围分别为0.20~0.94、0.56~0.94、1.43~3.30、0.13~0.58、0.87~1.36、0.53~1.57 mg·g^-1,经方法学考察,各成分呈现良好的线性关系,平均回收率在95.75%~101.6%之间,RSD在0.33%~1.06%之间。结论建立的HPLC指纹图谱和多指标含量测定方法稳定、可靠,可为壁钱药材、饮片和焙壁钱的质量评价提供依据。

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	石丽
	焦阳
	周广涛
	汪冰
	崔伟亮
	刘丽
	许丽丽
	林永强

关键词 ：壁钱药材, 壁钱饮片, 焙壁钱, 指纹图谱, 聚类分析, 主成分分析, 含量测定

Abstract：OBJECTIVE To establish the HPLC fingerprints and multi-components determination method of Uroctea compactilis, and evaluate its quality combined with chemometrics. METHODS Using Waters Symmetry RP-C₁₈ column, methanol as mobile phase A and 0.1% glacial acetic acid solution as mobile phase B, gradient elution(0-15 min, 0 A; 15-18 min, 0-10% A; 18-30 min, 10%-15% A)was carried out. The detection wavelength was set at 262 nm, the flow rate was 0.5 mL·min^-1 and the column temperature was maintained at 35 ℃. The fingerprints of 30 batches of Uroctea compactilis medicinal materials, decoction pieces of Uroctea compactilis and baked Uroctea compactilis were constructed. Combined with similarity analysis and chemometric analysis, the contents of uracil, guanine, hypoxanthine, uridine, inosine and guanosine were determined at the same time. RESULTS The similarity of fingerprints of 30 batches of Uroctea compactilis samples were more than 0.96. A total of 17 common peaks were calibrated and six chromatographic peaks were identified, namely uracil, guanine, hypoxanthine, uridine, inosine and guanosine. Cluster analysis divided 30 batches of Uroctea compactilis samples into three categories. Different processing specifications were grouped into one category. Principal component analysis showed that there were differences among Uroctea compactilis samples from different manufacturers, and there were little differences among Uroctea compactilis samples processed by different methods. The mass fractions of uracil, guanine, hypoxanthine, uridine, inosine, and guanosine were 0.20-0.94,0.56-0.94,1.43-3.30,0.13-0.58,0.87-1.36 mg·g^-1, and 0.53-1.57 mg·g^-1, respectively. Each component presented a good linear relationship, and the recovery was between 95.75%-101.6% and RSD was between 0.33%-1.06%. CONCLUSION The established HPLC fingerprint and multi index content determination method are stable and reliable, which can provide a basis for the quality evaluation of Uroctea compactilis, decoction pieces of Uroctea compactilis and baked Uroctea compactilis.

Key words： Uroctea compactilis decoction pieces of Uroctea compactilis baked Uroctea compactilis finger-print cluster analysis principal component analysis content determination

收稿日期: 2022-04-20

PACS:

R284

基金资助:山东省重点研发计划(软科学项目)资助(2020RKB24001);山东省人文社会科学课题资助(2021-YYGL-44);山东省中药材及饮片标准研究资助(2020-065,2020-066);中药配方颗粒质量识别与控制关键技术研究及产业化应用资助(2021CXGC010511)

通讯作者: 许丽丽,女,副主任药师研究方向:中药师中药质量评价及标准制修订 Tel:(0531)81216527;林永强,男,主任药师研究方向:中药质量控制及标准制修订 Tel:(0531)81216521

作者简介: 石丽,女,硕士研究生研究方向:药物分析

引用本文:

石丽, 焦阳, 周广涛, 汪冰, 崔伟亮, 刘丽, 许丽丽, 林永强. 基于指纹图谱结合化学计量学及多成分含量测定的壁钱质量研究[J]. 中国药学杂志, 2022, 57(22): 1935-1941. SHI Li, JIAO Yang, ZHOU Guang-tao, WANG Bing, CUI Wei-liang, LIU Li, XU Li-li, LIN Yong-qiang. Quality Study of Uroctea compactilis Based on Fingerprint Combined with Chemometrics and Multi-Component Content Determination. Chinese Pharmaceutical Journal, 2022, 57(22): 1935-1941.

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http://journal11.magtechjournal.com/Jwk_zgyxzz/CN/10.11669/cpj.2022.22.010 或 http://journal11.magtechjournal.com/Jwk_zgyxzz/CN/Y2022/V57/I22/1935

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