J. Cent. South Univ. Technol. (2007)03−0357−06
DOI: 10.1007/s11771−007−0071−7
Purification of chlorogenic acid in Flos Lonicerae with system of
polar ordered resins
XIANG Zhi-nan(向智男)
1
, ZHAN Yu(战 宇)
2
, NING Zheng-xiang(宁正祥)
1
(1. College of Light Industry and Food Science, South China University of Technology, Guangzhou 510640, China;
2.
School of Biological and Chemical Engineering, Guangzhou University, Guangzhou 510091, China)
Abstract: A system of polar ordered resins was established for purification of chlorogenic acid in Flos Lonicerae. It was composed
of three reversed phase resins, AB-8, DM-130 and NKA-9, representative for their gradually increased polarity and selectivity. A
method of RP-HPLC was used for determination of chlorogenic acid. And the performance of adsorption and desorption for
chlorogenic acid with the system of polar ordered resins was studied. Furthermore, the effects of concentration, pH and flow rate of
the adsorbate on adsorption ability were researched. It is indicated that the optimum parameters for chlorogenic acid are as follows:
pH 3.5 with a flow rate of 2.5 BV/h, the concentration of extract solution at 0.50, 0.40, 0.30 g/L respectively for the adsorptive
operation twice, and 6.93, 8.66, 10.39 mol/L ethanol used as gradient eluants. The purity of resulted product of chlorogenic acid
arrives 70.20% with yield of 89.79%. With simple procedures, low costs and high purity product, the method of system of polar
ordered resins followed by sequential reversed phase separations can be used to refine the chlorogenic acid in the extraction of Flos
Lonicerae.
Key words: chlorogenic acid; Flos Lonicerace; polar ordered adsorption and desorption; purification
1 Introduction
Flos Lonicerae (Honeysuckle Flower, JinYinHua in
Chinese), derived from the flower buds of several species
of the genus Lonicera (Cap-rifoliaceae), is a kind of
Chinese traditional medicine herb used in clinic for
centuries, such as the treatment of affection by
exopathogenic wind-heat or epidemic febrile diseases at
the early stage, sores, carbuncles, furuncles and
swellings
[1−2]
. It has medicinal efficiency of clearing
away heat and toxic materials, and is used to treat warm
diseases, dysentery due to damp-heat pathogen, and
carbuncle, etc
[3]
. Moreover, it can suppress the
N-nitrosating reaction and inhibit hepatic glucose
6-phosphatase
[4-6]
, which may be a significant factor in
diabetes. The results of chemical study showed that Flos
Lonicerae contains chlorogenic acid (a group of quinyl
ester of hydroxycinnamic acids abbreviated as CGA),
luteolin, lonicerin, inositol, etc. Among them, CGA is
considered as the main constituent that has antioxidant
activity
[7−8]
. Because of the certainty of curative effects,
CGA is now used not only as one of the quality control
in crude herbal drugs, but also in some preparations of
Chinese patent medicine and health food, in which the
extract of Flos Lonicerae is added
[9−10]
.
A number of conventional methods, such as
precipitation, extraction, crystallization and column
chromatography, were concerned on the CGA, among
which the tiptop purity just reached 36.28%
[11−12]
. An
ideal purity for chlorogenic acid from the crude extract
of Flos Lonicerae was achieved by high-speed-counter-
current chromatography (HSCCC). However, the
enormous cost and the complex operation for this
technology should be cognized, besides its low
productivity
[13]
.
Meanwhile, many scholars have done some work on
the resin adsorption for CGA. LIU and QIU
[14]
selected
NKA-Ⅱ resin as the absorbent to extract and purify
chlorogenic acid from leaves of Eucommia ulmoides,
with the adsorptive rate of 80.99%. LI et al
[15]
found
NKA-9 resin was the better one for purification of
chlorogenic acid when compared with resins X-5, AB-8
and S-8, with the purity of resulted product of 25.12%.
MA et al
[16]
chose the specific macorporous resin XDA-5
to adsorb and isolate chlorogenic acid and flavonoids,
and the content of purified chlorogenic acid in solid
extract was 36.65%. LI et al
[17]
introduced D
101
-column
separation-precipitation method for assaying chlorogenic
acid in Chinese medicinal preparations, and evaluated
that the D
101
resin could remove a great portion of
impurities.
Foundation item: Project(2005A20303002) supported by the Science and Technology Plan Item of Guangdong Province, China; Project (2006J1-C0251)
supported by the Science and Technology Bureau Foundation of Guangzhou, China
Received date: 2006−06−28; Accepted date: 2006−08−27
Corresponding author: XIANG Zhi-nan, PhD; Tel: +86-13533845658; E-mail: xiangwanzi2003@163.com