Identification of Volatile Components of Fresh Indocalamus Latifolius

Leaves by HS-SPME-GC-MS

Lingling Zhang

, Xiaofen Li

, Xiangpei Wang

, Yuqing Liang

, Xianyou Yang

, Hongmei Wu

Department of Pharmacognosy, Guiyang University of Chinese Medicine, 50, Nanming District, Guiyang City, Guizhou

Province, Guiyang 550002, PR China;

Kanong Yun Service Company Ltd of Guizhou Province, Zhenfeng County, Guizhou Province, Zhenfeng County,562201,

PR China

Keywords: fresh Indocalamus latifolius leaves; volatile compounds; GC-MS.

Abstract: The volatile components of fresh Indocalamus latifolius leaves were determined. They will provide

theoretical basis to develop and utilize the value of Indocalamus latifolius leaves. Headspace solid-phase

microextraction method (HS-SPME) with gas chromatography-mass spectrometry (GC-MS) was used for the

analyzing of volatile components from the fresh Indocalamus latifolius leaves. The relative percentage

proportions of volatile substances in sample were determined and compared. A total of 38 volatile

components were tentatively identified from fresh Indocalamus latifolius leaves by GC-MS, and the most

abundant compounds were cis-3-hexenol (33.893%), (E)-2-hexenal(20.461%), 1-hexanol (9.159%),

2-ethylfuran (4.923%), 1-penten-3-ol (2.224%) and hexanal(2.207%). The GC-MS method had the rapid,

simple and accurate advantages for the studying of the volatile components in fresh Indocalamus latifolius

leaves. It provides the basis for the further studies on the volatile components of Indocalamus latifolius

leaves.

1 INTRODUCTION

It is a traditional Chinese custom to eat rice

dumpling on Dragon Boat Festival in China for

thousands of years, and rice dumpling is also a kind

of festival food which is popular with the public. A

wide variety of rice dumpling leaves are the

indispensable materials for making this festival food,

and the south of China is generally dominated by

leaves of Indocalamus and Phrynium capitatum

Willd, while in the north of China the reed leaves

are used to make rice dumpling (Cen et al., 2017;

Wang, 2016). Among them, the leaves of

Indocalamus have been sourced for making rice

dumpling because it has wide and big leaf blade, as

well as its special scent. In addition, it has antiseptic

and sterilization effects (Xu and Xu, 1991). The

leaves of Indocalamus can be divided into

Indocalamus latifolius leaves, Indocalamus

tessellatus leaves, Indocalamus emeiensis leaves and

other 24 different varieties (Ai et al., 2004).

Shuifang Li et al demonstrated that its aroma was

associated with the volatile components in fresh

Indocalamus emeiensis and Indocalamus tessellatus

leaves, and the antiseptic effects of Phrynium

capitatum Willd was mainly associated with the

volatile components with antioxidant and

bacteriostatic activity (Yu et al., 2002; Li et al., 2015;

Lai et al., 2013). The Indocalamus latifolius leaves

is one of the most common materials for making rice

dumpling, and only the volatile components of the

dry Indocalamus latifolius leaves were identified (Li

et al., 2007a; Li et al., 2007b). However, the fresh

leaves are often used to wrap rice dumpling. To our

knowledge, there is no relevant reports on the

volatile components of fresh Indocalamus latifolius

leaves. Therefore, GC-MS was used to analyze the

volatile components of fresh Indocalamus latifolius

leaves in this study and the results provided

scientific basis for elucidating the chemical

substance base of the volatile components of fresh

Indocalamus latifolius leaves. It will provide

theoretical basis and technology indorsation for the

further promotion of Indocalamus latifolius leaves.

Zhang, L., Li, X., Wang, X., Liang, Y., Yang, X. and Wu, H.

Identiﬁcation of Volatile Components of Fresh Indocalamus Latifolius Leaves by HS-SPME-GC-MS.

DOI: 10.5220/0008184600100013

In The Second International Conference on Materials Chemistry and Environmental Protection (MEEP 2018), pages 10-13

ISBN: 978-989-758-360-5

2 EXPERIMENRAL

2.1 Materials

The fresh leaves of Indocalamus latifolius were

purchased from Beijing Hualian Supermarket in

Guiyang City, Guizhou Province, and has been

identified as Indocalamus latifolius by Professor

Xiangpei Wang of Guiyang University of Traditional

Chinese Medicine. The fresh leaves were cut into

small pieces, they were put in storage bags, and the

bags were kept in the refrigerator at -20℃.

2.2 Solid-phase Micro Extraction

Procedure

The sample was accurately weighed (0.5g) and

placed into 25 ml sample vial. Then, a 2cm-50/30um

DVB/CAR/PDMS Stable Flex fiber(American

Supelco company) was used to the headspace above

the sample for extracting 45 min under about 80℃.

The extraction head was removed from sample vial

and immediately inserted onto the GC injection

port,the sample thermal desorption for 3 min and

then directly injected into GC.

2.3 Gas Chromatography–Mass

Spectrometry Analysis

The analyses of gas chromatography was performed

on an HP6890/5975C (Agilent USA) using a

ZB-5MSi (5% phenyl-95% dimethylpolysiloxane)

fused silica capillary column, The pre-column

pressure was 7.62psi. The GC oven temperature was

programmed to hold at 40℃ for 2 min and then to

increase to 260℃ at 5℃ / min, running 46min. The

injector temperature were set at 250℃. High purity

helium (purity 99.999%) was used as carrier gas

with a flow rate of 1.0ml / min, samples were

injected in splitless mode. The solvent delay was

1min.

The Aglient 5975C mass spectrometer was

operated in the electron impact (EI) mode using an

ionisation energy at 70eV with a quadrupole

temperature set of 150℃ and a ionisation source

temperature of 230℃. The multiplier voltage was

1671V, the interface temperature was 280℃, the

emission current was 34.6μA and mass range was

29-500 amu.

2.4 Data Analysis

The peaks in the total ion flow map were retrieved

by the mass spectrometer computer data system and

identified by comparison to reference mass spectra

in the Nist2005 and Wiley275 databases. The

instrument Chemstation data processing system was

used to determine the relative concentrations of the

analytes by the peak area normalization method.

3 RESULTS

The volatile components were isolated and

identified(Table 1). The total ion chromatogram of

fresh Indocalamus latifolius leaves is shown in

Figure 1, and the corresponding volatile compounds

are listed in Table 1. A total of 38 volatile

components were tentatively identified in fresh

Indocalamus latifolius leaves by GC-MS, including

8 alcohols compounds (47.453%), 11 aldehydes

(28.202%), 7 terpenes (12.072%), 7 hydrocarbons

(0.692%), esters only detected cis-3-hexenyl acetate

(0.456%), heterocyclic detected 2-ethylfuran

(4.923%) and 2-amylfuran (0.102%), aromatic

detected benzaldehyde (1.593%) and

benzeneacetaldehyde (0.925%), alcohol components

mainly cis-3-hexenol (33.893%) and 1-hexanol

(9.159%), aldehyde components is dominated by

(E)-2-hexenal (20.461%), terpene component

mainly neophytadiene (9.463%), and the relative

percentage proportions of hydrocarbons were low.

Time(min)

Figure 1: TIC of volatile components extracted from fresh Indocalamus latifolius leaves.

5.0 0 10 .00 15 .0 0 20 .00 25 .0 0 30 .00 3 5.0 0 40 .0 0

10 00 000

20 00 000

30 00 000

40 00 000

50 00 000

60 00 000

70 00 000

T ime -->

Ab un dan ce

T IC: 1 70 526 06 .D

Identiﬁcation of Volatile Components of Fresh Indocalamus Latifolius Leaves by HS-SPME-GC-MS

Table 1: Percentages of volatile components extracted from fresh Indocalamus latifolius leaves.

No.

Retention time

Volatlie components

Relative percentage proportions (%)

1.75

ethanal

0.19

1.86

ethanol

0.04

2.08

1,3-pentadiene

0.02

2.19

isobutanal

0.21

2.42

butanal

0.04

2.72

isobutyl alcohol

0.01

2.94

3-methylbutanal

0.63

3.05

2-methylbutanal

0.89

3.33

1-penten-3-ol

2.22

3.54

2-ethylfuran

4.92

4.76

(E)-2-pentenal

0.04

5.00

1-pentanol

0.01

5.07

(Z)-2-pentenol

1.37

5.50

hexanal

2.20

7.07

(E)-2-hexenal

20.5

7.37

cis-3-hexenol

33.9

7.64

1-hexanol

9.15

9.19

(E,E)-2,4-hexadienal

1.63

10.58

benzaldehyde

1.59

11.19

2-amylfuran

0.10

11.7

cis-3-hexenyl acetate

0.45

12.47

(E,E)-2,4-heptadienal

0.29

13.15

benzeneacetaldehyde

0.92

14.47

linalool

0.73

14.65

nonanal

1.57

17.42

dodecane

0.01

17.77

2,6-dimethylundecane

0.15

18.00

beta.-cyclocitral

0.61

22.21

farnesane

0.06

22.85

tetradecane

0.14

23.67

alpha.-ionone

0.87

25.08

trans-.beta.-farnesene

0.06

25.15

beta.-ionone

0.85

25.33

pentadecane

0.22

25.65

E,E-.alpha.-farnesene

0.13

27.71

hexadecane

0.11

29.96

heptadecane

0.02

32.92

neophytadiene

9.46

MEEP 2018 - The Second International Conference on Materials Chemistry and Environmental Protection

4 CONCLUSIONS AND

DISCUSSION

The experimental results show that the main volatile

components of fresh Indocalamus latifolius leaves

were aromatic, heterocyclic, aldehydes, alcohols and

terpenes, among them, the relative percentage

proportions of cis-3-hexenol and (E)-2-hexenal were

the most abundant, As we know, cis-3-hexenol

mainly confers the aroma of herbs and green leaves,

while (E) -2-hexenol mainly exert an aroma of fresh

fruit (Li, 2007). These ingredients may play an

important role in the overall aroma of fresh

Indocalamus latifolius leaves. The relative

percentage proportions of alcohols, aldehydes and

terpenes were the greatest among the volatile

components of fresh Indocalamus latifolius leaves,

and (E)-2-hexenal resulted the most abundant

aldehyde. Terpenes and alcohols have been reported

to have strong antibacterial effects, and (E) -2-

hexenal has good inhibitory activity against bacteria

and fungal pathogens (Wang et al., 2018; Feng,

2010). These ingredients may play an important role

in rice dumpling having a longer shelf life. The

results indicate that fresh Indocalamus latifolius

leaves has good application prospects in the field of

antiseptic materials and food packaging. Based on

the exploration of volatile components of fresh

Indocalamus latifolius leaves, the purpose of this

article is to provides theoretical basis to develop and

utilize the value of Indocalamus latifolius leaves.

ACKNOWLEDGEMENTS

This work was supported by the Plan Project of

Science and Technology in Southwest Guizhou, PR

China (2016, NO.1-101), and Construction Project

of First-Class Discipline in Guizhou, PR China(2017,

NO.008). The authors thank the government of

China for their financial support.

REFERENCES

Ai, W.S., Li, C.Z., Chen, M.H., 2004. Hunan Forestry

Science Technology, 4(31): 15-17.

Cen, A.L., Deng, W., Mo, X.L., 2017. Seed, 36(1): 60-63.

Feng, G.H., 2010. ShangDong University Master's Thesis.

Lai, X., Wang, J.L., Ceng, D., 2013. Agricultural Science

in Guangdong, (9): 86-89.

Li, R., Hu, H.B., Li, X.F., 2015. Food Control, (51): 9-14.

Li, S.F., Wen, R.Z., Ceng, D., 2007a. Chinese Journal of

Chromatography, 25(1): 53- 57.

Li, S.F., Wen, R.Z., Ceng, D., 2007b. Journal of Chinese

Mass Spectrometry Society, 2(28): 117-122.

Li, X.Y., 2007. Beijing:Chemical Industry Press.

Wang, L., 2016. Food and Health, (6): 10-11.

Wang, Y.Q., Yang,Y.Z., Wu, Z.F., 2018. Chinese

Traditional and Herbal Drugs, 2(49): 455-461.

Xu, F., Xu, Z.M., 1991, Beijing: People's Medical

Publishing House, 32.

Yu, A.N., Wang, F.S., Yang, C.H., 2002. Fine Chemicals,

4(19): 201-202.

Identiﬁcation of Volatile Components of Fresh Indocalamus Latifolius Leaves by HS-SPME-GC-MS