目的 建立栀子的指纹图谱，并同时建立其中6个主要成分含量的一测多评分析方法，以期对栀子药材进行整体质量控制。方法 基于高效液相色谱结合紫外变波长分段检测，在各类化合物的最大吸收波长下，建立包含环烯醚萜苷类（240 nm）及二萜类（440 nm）成分信息的栀子指纹图谱。在此基础上，分别以栀子苷和西红花苷I为内标，计算4个环烯醚萜苷类成分（山栀苷、山栀子苷B、京尼平龙胆双糖苷和栀子苷）和2个二萜类成分（西红花苷I和西红花苷II）的校正因子，通过4台高效液相色谱仪及4根不同色谱柱进行耐用性考察，并与外标法测定结果比较，验证一测多评方法的准确性。结果 19批栀子的指纹图谱共标定20个共有峰，相似度为0.981～0.999；在240 nm下，以栀子苷为内标，山栀苷、山栀苷B、京尼平龙胆双糖苷和栀子苷的校正因子分别为1.15、1.36、1.54和1.00；440 nm下，以西红花苷I为内标，西红花苷II的相对校正因子为1.11，且耐用性较好。应用一测多评法测定6个成分的含量，与外标法测定结果比较，含量准确度均值为100.14%，RSD＜3%，无明显差异。19批栀子中6个待测成分的质量分数范围分别为0.09%～0.35%、0.28%～0.82%、0.31%～1.00%、4.60%～7.78%、0.62%～1.64%和0.07%～0.26%。结论 所建立的指纹图谱结合一测多评法简便可行，可为栀子药材整体质量控制提供一定参考和依据。

Objective To establish the fingerprint of Zhizi (Gardeniae Fructus) and a single standard for determination of multiple components (SSDMC) method to determine the content of six main components simultaneously, in order to control the overall quality of Gardeniae Fructus. Methods High performance liquid chromatography (HPLC) combined with ultraviolet (UV) variable wavelength detection was established. Under the maximum absorption wavelength of various compounds, the fingerprints of Gardeniae Fructus with the composition information of iridoid glycosides (240 nm) and diterpenoids (440 nm) were established. On this basis, with geniposide and crocin I as internal standards, calculating relative correction factors of four iridoid glycosides (shanzhiside, gardenoside B, genipin-1-β-D-gentiobioside and geniposide) and two diterpenoid components (crocin I and crocin II) to establish SSDMC method. Durability inspection through four high performance liquid chromatographs and four different chromatographic columns, and compared with the results of external standard method (ESM) to verify the accuracy of this method. Results A total of 20 common peaks were calibrated in fingerprints of 19 batches of Gardenia Fructus, the similarities of each batch were 0.981-0.999. At 240 nm, with geniposide as the internal standard, the correction factors of shanzhiside, gardenoside B, genipin-1-β-D-gentiobioside and geniposide were 1.15, 1.36, 1.54 and 1.00, respectively; at 440 nm, with crocin I as the internal standard, the relative correction factor of crocin II was 1.11, with good durability. The determined results of six components using SSDMC method were compared with the results of the ESM, and the results showed that the mean value of the accuracy of the content was 100.14% with RSD<3%, without significantly different. The content range of six components in 19 batches of Gardeniae Fructus were 0.09%-0.35%, 0.28%-0.82%, 0.31%-1.00%, 4.60%-7.78%, 0.62%-1.64% and 0.07%-0.26%, respectively. Conclusion The established fingerprint combined with SSDMC method are simple and feasible, which can provide some reference and basis for the overall quality control of Gardeniae Fructus.

R286.2

国家重点研发计划项目(2018YFC1707900)