不同干燥方式对连翘花主要成分的影响

杨梦婷1＊，王　相1，2，3，王倩 王鑫国 毕晓东 牛丽颖

中圖分类号 R284.1 文献标志码 A 文章编号 1001-0408（2021）08-0921-06

DOI 10.6039/j.issn.1001-0408.2021.08.05

摘 要 目的：建立测定阴干、真空冷冻干燥、烘箱干燥（30、50、70 ℃）、晒干等干燥方式下连翘花中4种成分含量的方法并进行比较，以评价不同干燥方式对连翘花主要成分含量的影响，筛选其最佳干燥方式。方法：采用超高效液相色谱法。色谱柱为Waters ACQUITY UPLC BEH C18，流动相为乙腈-0.1%磷酸水溶液（梯度洗脱），流速为0.3 mL/min，检测波长为230 nm，柱温为35 ℃，进样量为1 μL。采用优劣解距离法（TOPSIS）综合分析法计算不同干燥方式与理想方法的欧氏贴近度（Ci），以确定最佳干燥方法。结果：连翘酯苷A、芦丁、连翘酯苷、（+）-松脂素-4-O-β-D-葡萄吡喃糖苷检测进样量的线性范围分别为0.007 5～0.037 7、0.027 4～0.137 2、0.001 9～0.009 5、0.005 6～0.028 8 ?g（r均大于0.999）;精密度、稳定性（32 h）、重复性试验的RSD均小于2%;加样回收率分别为97.27%～102.53%、100.53%～104.11%、98.45%～104.02%、98.66%～104.82%，RSD均小于3%（n=3）。含量分别为1.645 8～4.987 9、11.730 2～20.978 0、0.875 5～2.005 0、2.366 0～5.535 7 mg/g。连翘酯苷A以30 ℃烘箱干燥后含量最高，芦丁、（+）-松脂素-4-O-β-D-葡萄吡喃糖苷均以真空冷冻干燥后含量最高，连翘苷以50 ℃烘箱干燥后含量最高。TOPSIS分析结果显示，阴干、真空冷冻干燥、烘箱干燥（30、50、70 ℃）、晒干的Ci分别为0.079 9、0.553 5、0.495 4、0.503 8、0.157 9、0.217 2;Ci排序为真空冷冻干燥>50 ℃烘箱干燥>30 ℃烘箱干燥>晒干>70 ℃烘箱干燥>阴干。结论：所建含量测定方法简便、重复性好，可用于同时测定连翘花中4种成分的含量。连翘花样品以真空冷冻干燥方式最佳，其次为50 ℃烘箱干燥、30 ℃烘箱干燥，再次为晒干和烘箱干燥70 ℃，最后为阴干。

关键词 连翘花;主要成分;阴干;烘箱干燥;真空冷冻干燥;晒干

Effects of Different Drying Methods on the Main Components of Forsythia suspensa Flowers

YANG Mengting1，WANG Xiang1，2，3，WANG Qian1，WANG Xinguo1，2，3，BI Xiaodong1，2，3，NIU Liying1，2，3（1. College of Pharmacy， Hebei University of TCM， Shijiazhuang 050091， China; 2. Hebei TCM Formula Granule Technology Innovation Center， Shijiazhuang 050091， China; 3. Hebei TCM Quality Evaluation and Standardization Engineering Research Center， Shijiazhuang 050091， China）

ABSTRACT   OBJECTIVE： To establish the method for the content determination of 4 components in Forsythia suspensa flowers by drying in shade， vacuum freeze-drying， oven （30， 50， 70 ℃） and sun， so as to evaluate the effects of different drying methods on the main components of F. suspensa flowers and screen the optimal drying method. METHODS： UPLC method was adopted. The determination was performed on Waters ACQUITY UPLC BEH C18 column with mobile phase consisted of acetonitrile-0.1% phosphoric acid aqueous solution （gradient elution） at the flow rate of 0.3 mL/min. The detection wavelength was set at 230 nm， and column was 35 ℃. The sample size was 1 μL. Euclidean closeness （Ci） of different drying methods was calculated by TOPSIS comprehensive analysis method， and the optimal drying method was defined. RESULTS： The linear range of forsythiaside A， rutin， forsythin， （+）-pinoresinol-4-O-β-D-glucopyranoside were 0.007 5-0.037 7， 0.027 4-0.137 2， 0.001 9-0.009 5， 0.005 6-0.028 8 ?g（all r>0.999）. RSDs of precision， stability （32 h） and reproducibility tests were all lower than 2%. The recoveries were 97.27%-102.53%， 100.53%-104.11%， 98.45%-104.02%， 98.66%-104.82%， respectively; and all RSDs<3%（n=3）. The contents were 1.645 8-4.987 9， 11.730 2-20.978 0， 0.875 5-2.005 0， 2.366 0-5.535 7 mg/g. The content of forsythiaside A was the highest after drying at 30 ℃， rutin  and （+）-pinoresinol-4- O-β-D-glucopyranoside were the highest after vacuum freeze-drying， forsythiaside was the highest after drying at 50 ℃. Results of TOPSIS analysis showed that Ci of F. suspensa flowers by drying in shade， vacuum freeze-drying， oven （30， 50， 70 ℃） and sun were 0.079 9， 0.553 5， 0.495 4， 0.503 8， 0.157 9， 0.217 2， respectively; the order of Ci was vacuum freeze-drying> 50 ℃ oven drying> 30 ℃ oven drying>sun drying>70 ℃ oven drying> shade drying. CONCLUSIONS： Established method is simple， reproducible and can be used for the content determination of 4 components in F. suspensa flowers. The samples are preferably dried by vacuum freeze-drying， followed by 50 ℃ oven drying， 30 ℃ oven drying， and then dried in the sun and oven at 70 ℃ and finally in the shade.

KEYWORDS   Forsythia suspensa flowers; Main component; Drying in the shade; Oven drying; Vacuum freeze-drying; Drying in the sun

连翘为木犀科植物连翘Forsythia suspensa（Thunb.）Vahl的干燥果实，始载于《神农本草经》[1]，主产于我国山西、河南、陕西、湖北等省，具有清热解毒、消肿散结、疏散风热之功效，主要含有苯乙醇类、木质素类、黄酮类、三萜酸类、挥发油类等成分[2]。《本草纲目》中记载，……