不同干燥方式对连翘花主要成分的影响

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1μL。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0.0075~0.0377、0.0274~0.1372、0.0019~0.0095、0.0056~0.0288μg(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1.6458~4.9879、11.7302~20.9780、0.8755~2.0050、2.3660~5.5357 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0.0799、0.5535、0.4954、0.5038、0.1579、0.2172;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。

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

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 1μL.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 0.0075-0.0377,0.0274-0.1372,0.0019-0.0095,0.0056-0.0288μg(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 1.6458-4.9879,11.7302-20.9780,0.8755-2.0050,2.3660-5.5357 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 0.0799,0.5535,0.4954,0.5038,0.1579,0.2172,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.