全 文 ：Determination of Five Metallic Elements in
Guoshangye from Guizhou by Microwave
Digestion-flame Atomic Absorption Spectrometry
Sibu MA1,2, Shaohui WANG2, Tongxiang LIU2*, Kaibing LI3, Wei CHEN3
1. Minzu University of China, Beijing 100081, China;
2. GuiYang college of Traditional Chinese Medicine, Guiyang 550002, China;
3. Anshun Institute for Food and Drug Control, Anshun 561000, China
Supported by the Research Project for Postgraduate Students of Minzu University of
China in 2015; Scientific and Technological Cooperation Planning Project of Guizhou
Province (QKJ LH[2015]7265).
*Corresponding author. E-mail: liutongxiang6168@sina.com
Received: September 10, 2015 Accepted: December 14, 2015A
Agricultural Science & Technology, 2016, 17(2): 262-264
Copyright訫 2016, Information Institute of HAAS. All rights reserved Agricultural Basic Science and Technology
G uoshangye is dry rhizome andpseudobulb of Pholidota yun-nanensis Rolfe in Orchi-
daceae used by ethnic minorities in
Guizhou, and recorded in “Guizhou
Traditional Chinese Medicinal Material
and Ethnic Minority Medicine Quality
Standard” (2003 Edition). Gu-
oshangye has the effects of nourishing
yin to clear away the ling-heat, pre-
venting phlegm from forming and
stopping cough, and promoting qi cir-
culation to relieve pain, and is used for
treating cough caused by phthisis,
hemoptysis, chronic tracheitis, chronic
pharyngitis, colic pain, irregular men-
struation and pain caused by skin and
external diseases widely in Guizhou
individually. Modern studies indicated
that Guoshangye had a stronger inhi-
bition effect on NO generation by
macrophages of rats and a blocking
effect on cell cycle of human liver
cancer HepG2 cells. Besides organic
compounds in it as effective compo-
nents, existed inorganic metallic ele-
ments often play a role of enhancing
the efficacy of Guoshangye. In this
study, Guoshangye from Guizhou was
subjected to microwave digestion, and
five metallic elements in it were deter-
mined by flame atomic absorption
spectroscopy.
Materials and Methods
Experimental material
Guoshangye was collected from
Kaili City of Guizhou Province, and i-
dentified by associate professor Sun
Qingwen from Department of Phar-
macognosy of Guiyang University of
Traditional Chinese Medicine as
Pholidota yunnanensis Rolfe in Orchi-
daceae, and the voucher specimen
was stored in Anshun Institute for
Food and Drug Control of Guizhou
Province (serial number: YNSXT-01).
Instruments and Reagents
Instruments
Following instruments were used:
an AAnalyst 400 type atomic absorp-
tion spectrophotometer (PerkinElmer,
Abstract In the study, the contents of 5 trace elements including Fe, Cu, Mg, Mn
and Ca were directly analyzed by flame atomic absorption spectroscopy in Gu-
oshangye. The sample was subjected to microwave digestion with HNO3 and H2O2,
and detected by the standard curve method. The results showed that Guoshangye
contained abundant trace elements which were necessary for human. The recovery
rates of these trace elements were in the range of 96%-103%. The method is ac-
curacy and satisfactory.
Key words Trace elements; Guoshangye; Flame atomic absorption spectroscopy
微波消解-火焰原子吸收光谱
法测定黔产果上叶中 5 种金属
元素的含量
马四补 1,2，王绍辉 1，刘同祥 1*，李开斌 3，陈维 3
（1. 中央民族大学，北京 100081；2. 贵阳中
医学院，贵州贵阳 550002；3. 安顺市食品药品
检验所，贵州安顺 561000）
摘 要 [目的]测定黔产果上叶中 5 种金属元
素的含量。 [方法]运用火焰原子吸收光谱法测
定果上叶中 Fe、Cu、Mg、Mn 和 Ca 5 种金属元
素，采用浓硝酸-双氧水微波消解样品，标准曲
线法检测回收率。 [结果]所测定的果上叶中含
有丰富的人体必须金属元素， 回收率在 96％～
103％。 [结论]该方法准确易行，结果令人满意。
关键词 微量元素;果上叶;原子吸收分光光度
法
基金项目 2015 年中央民族大学研究生科研
项目 民族药果上叶乙酸乙酯提取部位化学成
分研究；贵州省科技合作计划项目（项目编号：
黔科合 LH 字[2015]7265 号）。
作者简介 马四补（1979-），男，贵州威宁人 ，
副教授，在读博士，从事民族医药研究，E-mail：
453175568@qq.com。*通讯作者，教授， E-mail：
liutongxiang6168@sina.com。
收稿日期 2015-09-10
修回日期 2015-12-14
DOI:10.16175/j.cnki.1009-4229.2016.02.005
Agricultural Science & Technology2016
Table 4 Results of recovery test of the five elements in Guoshangye
Element Amount in sampleμg
Added standard
μg
Measured
amount//μg Recovery rate//%
Iron 2.90 3.00 5.73 97.2
Copper 1.52 1.50 2.92 96.6
Magnesium 14.69 15.00 30.35 102.2
Manganese 5.12 5.00 9.81 96.9
Calcium 65.53 60.00 123.31 98.2
Table 2 Determination conditions for elements including iron
1 2 3 4 5
Lamp current//mA 10 6 15 10 6
Lamp current//mA 248.3 324.8 285.2 279.5 309.3
Slit//nm 0.5 0.5 0.7 0.2 0.8
Carrier gas//ml/min 200 200 200 200 200
Injection volume//μl 10 10 10 10 10
Graphite furnace Tube type Tube type Tube type Tube type Tube type
Determination mode Peak area Peak area Peak area Peak area Peak area
America); Fe, Cu, Mg, Ca and Mn
hollw cathode lamps (Beijing General
Research Institute For Non-ferrous
Metals); and a WX-4000 type rapid
microwave digester (Shanghai Yiyao
Analytical Instrument Co. Ltd).
Reagents
Fe (GBW (E)080123-14032), Cu
(GBW(E)080122-14062, Mg (GBW(E)
080262-13032), Ca (GBW(E)080261-
14091) and Mn (GBW (E)080263-
10042) standard solutions with a con-
centration of 1 000 μg/ml were provid-
ed by National Research Center for
Certified Reference Material; used
water was ultrapure water, and used
nitric acid was GR grade (Chengdu
Jinshan Chemical Reagent Co., Ltd.);
and hydrogen peroxide was GR grade
(Sinopharm Chemical Reagent Co.,
Ltd.). All used apparatuses were
cleaned and treated according to the
requirement by atomic absorption
spectroscopy.
Experimental methods
Preparation of standard solutions
The nitric acid was diluted into a
0.5% nitric acid solution as a diluent for
preparing the standard solutions of the
five elements, and the concentrations
were shown in Table 1.
Sample treatment
Guoshangye was cut longitudinal-
ly into slices, which were dried in a
vacuum drying oven for 12 h at 85 ℃,
pulverized, and stored in a dryer.
Sample digestion
Above powder (0.500 0 g) was
accurately weighed and added in a
clean microwave digestion tank, into
which added concentrated nitric acid
(4 ml) and hydrogen peroxide (1 ml)
were, microwave digestion was con-
ducted under an airtight condition, and
a blank experiment was performed si-
multaneously. After the microwave di-
gestion, the solution was pale yellow
and was evaporated to nearly dry, the
residue was dissolved with diluted ni-
tric acid and transferred into a 25 ml
volumetric flask, the digestion tank
was cleaned with the 0.5% nitric acid
solution which was then added into the
volumetric flask, and the solution in the
volumetric flask was diluted to con-
stant volume as a sample solution.
Results and Analysis
Establishment of determination
conditions and standard equations
for the five elements
The atomic absorption spec-
trophotometer was set according to its
operation steps and the prepared
standard solutions, and the instrument
parameters in the experiment were
shown in Table 2. Sample injection
was performed according to concen-
trations in Table 1, respectively, to de-
termine peak areas, which were then
used for construction of operation eq-
uations together with the concentra-
tions. The fourth injected standard so-
lution was subjected to sample injec-
tion for 5 times for the determination of
peak areas, and the result showed a
RSD value less than 5% , indicating
that the instrument had good preci-
sion.
Determination results
Parallel samples (n=5) were de-
termined according to the experimen-
tal conditions in Table 2 for peak ar-
eas, and contents of the five metallic
elements in Guoshangye were calcu-
lated and converted into mg/kg. The
results were shown in Table 3.
Recovery test
In order to verify the accuracy of
this experiment and the feasibility of
the method, this study performed a re-
covery test, and the result in Table 4
showed that the recovery of the five
elements was in the range of 96% -
103%, indicating that the experimental
results were accurate and reliable, and
the method of this experiment was fea-
sible.
Conclusions and Discus-
sion
Guoshangye produced in
Guizhou is rich in five essential trace
elements for human, the contents of
Mg, Mn and Ca in it were higher than
common plants, and contents of Fe
Table 1 Series standard solutions of the five elements ng/ml
Trace element 1 2 3 4 5 6
Fe 10 20 40 60 80 100
Cu 20 40 80 120 180 200
Mg 10 20 40 60 80 100
Mn 10 20 40 60 80 100
Ca 10 20 40 60 80 100
Table 3 Determination results of five metallic elements in Guoshangye
Element Content//mg/kg RSD value//% (n=5)
Iron 14.55 1.62
copper 6.00 0.76
Magnesium 70.05 1.32
Manganese 46.86 1.15
Calcium 1 356.12 1.63
263
Agricultural Science & Technology 2016
Responsible editor: Tingting XU Responsible proofreader: Xiaoyan WU
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and Cu were higher as well. Cu, Fe,
Mg, Mn and Ca play different roles in
human metabolism: Cu participates in
metabolism of various enzymes, syn-
thesis of noradrenaline and regulation
of blood pressure; Fe participates in
hematopoiesis as well as synthesis of
hemoglobin and myohemoglobin for
transport and storage of oxygen in vi-
vo, and serves as the active center of
a variety of enzymes; and Ca has the
effects of reducing blood pressure and
lowering incidence of stroke. The effi-
cacy of Guoshangye is related to
these inorganic metallic elements,
which do not directly participate in the
efficacy of organic compounds, but
could improve enzyme activities in vivo
as well as human immunity, supple-
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human body, and also serve as one
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