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1.重庆三峡学院 生物与食品工程学院 三峡库区道地药材绿色种植与深加工重庆市工程实验室, 重庆 404000
2.重庆市万州食品药品检验所,重庆 404000
3.重庆三峡医药高等专科学校 中医学院,重庆 404120
黄小兰,在读硕士,工程师,从事药用植物资源的开发与利用研究,E-mail:534832723@qq.com
郭冬琴,博士,副教授,从事药用植物栽培与质量控制研究,Tel:023-58102130,E-mail:guodongqin1997@163.com; *
周浓,硕士,教授,从事药用植物栽培与质量控制研究,Tel:023-58576130,E-mail:erhaizn@126.com
修回日期:2019-12-12,
网络出版日期:2020-06-09,
纸质出版日期:2020-08-05
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黄小兰,何旭峰,杨勤等.HPLC-PDA同时测定地笋中7种酚酸的含量[J].中国实验方剂学杂志,2020,26(15):156-162.
HUANG Xiao-lan,HE Xu-feng,YANG Qin,et al.Simultaneous Determination of 7 Phenolic Acids in Lycopus lucidus var. hirtus Rhizome by HPLC-PDA[J].Chinese Journal of Experimental Traditional Medical Formulae,2020,26(15):156-162.
黄小兰,何旭峰,杨勤等.HPLC-PDA同时测定地笋中7种酚酸的含量[J].中国实验方剂学杂志,2020,26(15):156-162. DOI: 10.13422/j.cnki.syfjx.20201615.
HUANG Xiao-lan,HE Xu-feng,YANG Qin,et al.Simultaneous Determination of 7 Phenolic Acids in Lycopus lucidus var. hirtus Rhizome by HPLC-PDA[J].Chinese Journal of Experimental Traditional Medical Formulae,2020,26(15):156-162. DOI: 10.13422/j.cnki.syfjx.20201615.
目的
2
建立同时测定地笋中丹参素、原儿茶酸、原儿茶醛、绿原酸、咖啡酸、阿魏酸和迷迭香酸7种酚酸的高效液相色谱-二极管阵列检测法(HPLC-PDA),并对不同产地地笋中酚酸类成分进行分析评价。
方法
2
样品采用80%甲醇超声提取,采用资生堂CAPCELL PAK C
18
色谱柱(4.6 mm×250 mm,5 μm);流动相甲醇-0.02%甲酸水溶液(pH 3.0)梯度洗脱;检测波长279,324 nm;柱温30 ℃;流速1.0 mL·min
-1
;进样体积20 μL。
结果
2
7种酚酸成分在各自的质量浓度范围内线性关系良好(
r
≥0.999 9),平均回收率96.49%~103.45%,RSD 0.5%~2.8%,检出限(S/N=3)0.008~0.046 mg·L
-1
,定量限(S/N=10)0.027~0.154 mg·L
-1
。不同产地地笋均检出7种酚酸类成分,总质量分数5 811.01~11 747.23 µg·g
-1
,平均质量分数7 421.05 µg·g
-1
,不同种酚酸类化合物含量存在较大差异,其中各产地均以迷迭香酸含量最高,平均值7 111.19 µg·g
-1
,占酚酸总量的95.8%,为地笋酚酸的主要成分;主成分分析和聚类分析结果均显示产地为山东菏泽的地笋质量较优,其次为重庆万州。
结论
2
该方法操作简便、灵敏度高、准确性好、实用可靠,适用于地笋酚酸的含量测定,以期为地笋药材质量标准和产品开发提供参考。
Objective
2
A high performance liquid chromatography-photo-diode array(HPLC-PDA) method for the simultaneous determination of the 7 phenolic acids including danshensu,protocatechuic acid,protocatechuic aldehyde,chlorogenic acid,caffeic acid,ferulic acid and rosemary acid in
Lycopus lucidus
var.
hirtus
rhizome,analyzing and evaluating the phenolic acids in
L.lucidus
var.
hirtus
rhizome collected from different habitats,is reported here.
Method
2
The sample was extracted by ultrasonic with 80% methanol solution,7 kinds of phenolic acids were separated on a CAPCELL PAK C
18
column (4.6 mm×250 mm,5 μm) with a mobile phase consisting of methanol-0.02% formic acid aqueous (pH 3.10)by gradient elution,The detection wavelength was at 279,324 nm, the column temperature was 30 ℃ with 20 μL injection volume and the flow rate was 1.0 mL·min
-1
.
Result
2
The 7 Phenolic acids had a good linear relationship (
r
≥0.999 9) within their respective mass concentration ranges,the average recovery was 96.49%-103.45% and the RSD was 0.5%-2.8%,the limit of determination was 0.008-0.046 mg·L
-1
and the limit of quantification was 0.027-0.154 mg·L
-1
.The 7 kinds of phenolic acids were all detected in
L.lucidus
var.
hirtus
rhizome and the total amount was between 5 811.01 and 11 747.23 µg·g
-1
, the average amount was 7 421.05 µg·g
-1
.The content of 7 phenolic acids was different and the rosemary acid was the highest in all the samples with an average of 7 111.19 µg·g
-1
the ratio to the total phenolic acids was 95.8%.The results of principal component analysis and cluster analysis showed that the quality of
L.lucidus
var.
hirtus
rhizome from Heze city in Shandong province was better,followed by Wanzhou district in Chongqing.
Conclusion
2
The method was simple,sensitive,accurate,practical and reliable,and is suitable for the content determination of phenolic acid in
L. lucidus
var.
hirtus
rhizome.It is expected to provide a reference for the improvement of quality standard and a new idea for the development and utilization of
L.lucidus
var.
hirtus
rhizome.
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