HPLC法测定不同采收期香青兰中黄酮和酚酸类的含量

目的: 测定不同时期采收的香青兰药材中黄酮类成分(木犀草素-7-O-β-D-葡萄糖醛酸苷、芹菜素-7-O-β-D-葡萄糖醛酸苷、香叶木素-7-O-β-D-葡萄糖醛酸苷和田蓟苷)和酚酸类成分(迷迭香酸)的含量,确定最佳采收期。方法: 采用Purospher^® STAR LP RP-18 endcapped(4.6 mm×250 mm,5 μm)色谱柱,以乙腈(A)-0.5% 甲酸水溶液(B)为流动相,梯度洗脱(0~30 min,17%A;30~60 min,17%A→28%A;60~75 min,28%A),流速1.0 mL·min^-1,检测波长330 nm,柱温35 ℃。结果: 木犀草素-7-O-β-D-葡萄糖醛酸苷、芹菜素-7-O-β-D-葡萄糖醛酸苷、迷迭香酸、香叶木素-7-O-β-D-葡萄糖醛酸苷、田蓟苷5 种化学成分的分离效果良好,质量浓度在相应的范围内与峰面积有良好的线性关系,相关系数均大于0.999 5;平均加样回收率(n=6)为98.4%~99.5%(RSD<1.9%,n=6)。该方法应用于研究新疆吉木萨尔县产区不同采收期对香青兰药材中5 种化学成分含量的影响,本试验在6 月13 日(种植后213 d)至8 月6 日(种植后270 d)内设置了8 个采收期,发现木犀草素-7-O-β-D-葡萄糖醛酸苷等上述5 种化学成分的含量与采收期(种植后天数)均呈二次或三次函数关系,随着采收期的推迟,含量先增后减。结论: 该含量测定方法操作简单,重复性好,为确定香青兰药材适宜采收期提供依据。香青兰药材中木犀草素-7-O-β-D-葡萄糖醛酸苷等5 种化学成分含量随采收期不同而异,其总量最大值出现在7 月中上旬。

Objective: To simultaneously determine the contents of luteolin-7-O-β-D-glucuronide, apigenin-7-O-β-D-glucuronide,diosmetin-7-O-β-D-glucuronide,and tilianin(flavonoids)and rosmarinincacid(phenyl phenyl propanoids)of Dracocephalum moldavica L. ,so as to find out the best harvest time. Methods: HPLC was performed on a Purospher^® STAR LP RP-18 endcapped column(4.6 mm×250 mm,5 μm)at 35 ℃ with acetonitrile(A)-0.5% formic acid aqueous solution(B)as the mobile phase by gradient elution(0-30 min,17%A;30-60 min,17%A→28% A;60-75 min,28% A). The detection wavelength was 330 nm,and the flow rate was 1 mL·min^-1. Results: The baseline separation of these 5 components was achieved. The calibration curve was linear(r ≥ 0.999 5)over the tested ranges. The average recovery was 98.4%-99.5%(RSD<1.9%,n=6). The method has been successfully applied to the analysis of Dracocephalum moldavica in different harvest periods. In this paper,single-factor randomized block design was applied to study the 5 components content of Dracocephalum moldavica on eight collecting stages. For the Dracocephalum moldavica L. collected from June 13 to August 6,the contents of 5 ingredients increased primarily,and then decreased. Conclusion: The established method is proved to be simple and repeatable, which can provides the basis for the suitable harvest time of Dracocephalum moldavica . The contents of the 5 components are different in different harvest time. The maximum contents appear in the early of July.