摘要
目的建立栀子的超高效液相色谱(UPLC)指纹图谱及其分析方法,为其质量控制提供科学依据。方法采用UPLC可变波长测定法,Waters ACQUITY UPLC BEH C_(18)(2.1mm×50mm,1.7μm)色谱柱,流动相为乙腈-0.1%甲酸水,梯度洗脱;检测波长为238nm(0~5.4min),440 nm(5.4~10 min);体积流量为0.4 mL·min^(-1);柱温30℃;进样量2μL。通过相似度评价、主成分分析、偏最小二乘判别分析对16批栀子样品指纹图谱进行分析。结果建立了不同产地栀子的指纹图谱,标定了23个共有峰并指认了其中4个共有峰:京尼平龙胆双糖苷(4号峰)、栀子苷(6号峰)、西红花苷Ⅰ(15号峰)和西红花苷Ⅱ(17号峰)。16批样品相似度在0.9860~0.9950之间,通过主成分分析、偏最小二乘判别分析将不同产地栀子分为两组,浙江为一组(S1~S6),其余产地为一组(S7~S16),并发现京尼平龙胆双糖苷、西红花苷Ⅰ和西红花苷Ⅰ等11个差异较大的成分。结论不同产地栀子的UPLC指纹图谱的构建和化学模式的识别为浙江道地栀子的质量控制及品质评价提供了更全面的参考。
OBJECTIVE To establish the UPLC fingerprint of Gardeniae Fructus for providing reference for effective quality control. METHODS The samples were analyzed on a Waters ACQUITY UPLC BEH C18 （2. 1 mm × 50 mm, 1.7 μm） column maintained at 30 ℃ and eluted with methanol and water containing 0. 02% phosphoric acid as mobile phases in a linear gradient mode. The flow rate was set at 0. 4 mL . min-1 and the injection volume was 0. 2 μL. The detection wavelengths were set at 238 nm （0 - 5.4 min） and 440 nm （5.4 - 10 min）. RESULTS The fingerprints of 16 batches of samples were analyzed with similarity evaluation, principal component analysis （PCA） and partial least squares discriminant analysis （PLS-DA）. The common mode of the fingerprint was established with 24 common peaks, and four of them were identified, which were genipin 1-gentiobioside （4）, gardenoside （6）, crocin Ⅰ （15）, and crocin Ⅱ（17）. The similarity degrees of the 16 batches of samples were between 0. 986 0 and 0. 995 0. The samples were divided into two groups, ZheJiang （S1 -S6） and other areas （S7 -S16）, analyzed by principal component analysis （PCA） and partial least squares discriminant analysis （PLS-DA）. Eleven significantly different components were found, including genipinl-gentiobioside, gardenoside, crocin Ⅰ , crocin Ⅱand some others. CONCLUSION The establishment of UPLC fingerprint of Gardeniae Fructus from different producing areas and the application of chemical pattern recognition can provide more comprehensive references for the quality control and evaluation of genuine Gardeniae Fructus from Zhejiang Province.
出处
《中国药学杂志》
CAS
CSCD
北大核心
2017年第1期63-67,共5页
Chinese Pharmaceutical Journal
基金
国家中医药行业专项基金项目(2015468002-2)
国家科技基础性工作专项(2014FY111100)
江苏高校优势学科建设工程资助项目
关键词
栀子
指纹图谱
超高效液相色谱可变波长法
相似度评价
主成分分析
偏最小二乘分析
Gardeniae Fructus
fingerprint
variable wavelength method of ultra-performance liquid chromatography
similarity evaluation
principal component analysis
partial least squares discriminant analysis
