栀子类药材中西红花苷类成分的定性定量分析  

Qualitative and quantitative analysis on crocins in fruits of Gardenia species

作　　者：叶潇[1] 张东[1] 冯伟红[1] 梁曜华[1] 刘晓谦[1] 李春[1] 王智民[1] YE Xiao;ZHANG Dong;FENG Wei-hong;LIANG Yao-hua;LIU Xiao-qian;LI Chun;WANG Zhi-min(National Engineering Laboratory for Quality Control Technology of Chinese Herbal Medicines,Institute of Chinese Materia Medica China Academy of Chinese Medical Sciences,Beijing 100700,China)

机构地区：[1]中国中医科学院中药研究所中药质量控制技术国家工程实验室,北京100700

出　　处：《中国中药杂志》2022年第16期4377-4384,共8页China Journal of Chinese Materia Medica

基　　金：中国中医科学院科技创新工程项目(CI2021A04807)。

摘　　要：该文旨在对栀子和水栀子中的西红花苷类成分进行比较研究。采用Acchrom XCharge C_(18)色谱柱(4.6 mm×250 mm, 5μm)进行分离,流动相为乙腈和0.1%甲酸水溶液,梯度洗脱,检测波长440 nm,流速1.0 mL·min,柱温30℃。采用上述色谱条件对20批栀子和8批水栀子样品进行测定,建立了栀子中西红花苷类成分的HPLC指纹图谱;利用UHPLC-ESI-Orbitrap-MS/MS技术和对照品对共有峰进行结构推测和指认。结果28批样品中共选出20个共有峰,质谱推测了其中16个共有峰的结构,并经对照品比对确认了其中4个共有峰,分别是西红花苷Ⅰ、Ⅱ、Ⅲ和Ⅳ。采用同一色谱条件对西红花苷Ⅰ~Ⅳ进行了同步测定,系统适应性与方法学考察结果均符合含量测定要求。28批样品指纹图谱与对照指纹图谱的相对相似度均在0.98以上。但聚类分析结果显示,栀子和水栀子各聚为一组。20批栀子中西红花苷Ⅰ的质量分数在3.58~9.58 mg·g^(-1),西红花苷Ⅱ在0.230~1.452 mg·g^(-1),西红花苷Ⅳ在0.014 5~0.135 mg·g^(-1),西红花苷Ⅲ在0.301~1.12 mg·g^(-1),4种成分的总质量分数在4.12~12.25 mg·g^(-1);8批水栀子中西红花苷Ⅰ的质量分数在5.84~11.48 mg·g^(-1),西红花苷Ⅱ在0.308~0.898 mg·g^(-1),西红花苷Ⅳ在0.010 6~0.025 5 mg·g^(-1),西红花苷Ⅲ在0.675~1.34 mg·g^(-1),4种成分的总质量分数在6.97~13.72 mg·g^(-1)。现有结果表明栀子和水栀子在西红花苷类成分组成上存在一定相似性。该文所建方法为栀子、水栀子及相关产品的质量控制提供了参考。The aim of this study was to compare crocins in the fruit of Gardenia jasminoides and Gardenia jasminoides var. radicans. Acchrom XCharge C_(18)column(4.6 mm×250 mm, 5 μm) was used for separation, with mobile phase of acetonitrile and 0.1% formic acid for gradient elution. The detection wavelength was set at 440 nm with a flow rate of 1.0 mL·min, and the column temperature was 30 ℃. The high performance liquid chromatography(HPLC) fingerprint of crocin in Gardenia species was established by testing 20 batches of G. jasminoides and 8 batches of G. jasminoides var. radicans samples from different sources, and UHPLC-ESI-Orbitrap-MS/MS technology and reference substances were used to predict and identify the common peaks. The results showed that 20 common chromatographic peaks from the samples were selected and the structures of 16 common peaks were predicted by mass spectrum. Four common peaks(crocin Ⅰ, Ⅱ, Ⅲ, and Ⅳ) were identified by the comparison with reference substances. The content of crocin Ⅰ, Ⅱ, Ⅲ, and Ⅳ was determined simultaneously under the same chromatographic condition, and both the system suitability and the methodological investigation results met the requirements of content determination. The relative similarity of HPLC fingerprint of 28 samples to the reference fingerprint was above 0.98. The results of cluster analysis(CA) showed that G. jasminoides and G. jasminoides var. radicans were separately grouped into one group. In the 20 batches of G. jasminoides, the content of crocin Ⅰ, Ⅱ, Ⅳ, and Ⅲ was between 3.58-9.58, 0.230-1.452, 0.014 5-0.135, and 0.301-1.12 mg·g^(-1), respectively, and the total content was between 4.12-12.25 mg·g^(-1). In the 8 batches of G. jasminoides var. radicans, the content of crocin Ⅰ, Ⅱ, Ⅳ, and Ⅲ was between 5.84-11.48, 0.308-0.898, 0.010 6-0.025 5, and 0.675-1.34 mg·g^(-1), respectively, and the total content was between 6.97-13.72 mg·g^(-1). The existing results showed that there is a certain similarity between G. jasminoides and

关 键 词：栀子 水栀子 西红花苷 指纹图谱 含量测定 

分 类 号：R284.1[医药卫生—中药学]