Optimization of extraction and identification of volatile compounds from <i>Myrciaria floribunda</i>

García, Yesenia Mendoza; Lemos, Eurico Eduardo Pinto de; Augusti, Rodinei; Melo, Júlio Onésio Ferreira

doi:10.5935/1806-6690.20210031

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Scientific Article • Rev. Ciênc. Agron. 52 (3) • 2021 • https://doi.org/10.5935/1806-6690.20210031 copy

Optimization of extraction and identification of volatile compounds from Myrciaria floribunda¹ 1 Work extracted from the thesis of the first author, presented to the Graduate Program in Agronomy, Federal University of Alagoas/UFAL-AL

Otimização da extração e identificação dos compostos voláteis de Myrciaria floribunda

Authorship SCIMAGO INSTITUTIONS RANKINGS

ABSTRACT

The composition of the volatile profile of rumberry fruits (Myrciaria floribunda) was determined using solid- phase microextraction in headspace mode and gas chromatography, coupled with mass spectrometry. The PA (polyacrylate) and DVB/CAR/PDMS (divinylbenzene/carboxen/polydimethylsiloxane) fibers were optimized for the extraction parameters (agitation, extraction time and temperature), in order to select the fiber with the highest number of isolated compounds. A total of 48 volatile compounds were identified using HS-SPME/GC-MS present in the ripe fruits of rumberry. The volatile compounds were classified into five chemical classes, the majority belonging to the sesquiterpenes class (71%). In addition, it was possible to verify that the fiber coated with polyacrylate (PA) had better performance, allowing for the extraction of a greater number of volatile compounds (n = 35). The extraction conditions that allowed the isolation of a greater number of volatile compounds corresponded to times greater than 26 minutes and temperatures above 85 °C, with agitation of 79 rpm for the PA fiber. Likewise, it was found that the hydrocarbon sesquiterpenes was the chemical class most present in the fruits, which is mainly related to the volatile profile of rumberry fruits.

Key words:
Rumberry; Myrtaceae; Solid-phase microextraction

Variables	Levels of variation
Variables	-1	0	+1
Extraction time (min)	10	20	30
Adsorption temperature (°C)	30	65	100
Agitation (rpm)	0	50	100

Assay	Factors			Response Variables
Assay	Time (min)	Temperature (°C)	Agitation (rpm)	PA (%)	DVB/CAR/PDMS (%)
1	14	45	21	130660658	5712883,925
2	26	45	21	197421957	7884439,133
3	14	85	21	171669590	18991038
4	26	85	21	473628360	14316985,9
5	14	45	79	72949751	23487624,8
6	26	45	79	137765497	14074138,76
7	14	85	79	318966807	23841402,9
8	26	85	79	540193684	17013588,8
9	10	65	50	85949619	2763265,76
10	30	65	50	124736784	15844343
11	20	30	50	76694399	8766278,08
12	20	100	50	415749747	8365294,01
13	20	65	0	155937458	165076,265
14	20	65	100	174558957	20028526,6
15^* * Central points.	20	65	50	130723212	2107432,83
16^* * Central points.	20	65	50	116735828	9760817,99
17^* * Central points.	20	65	50	91195137	1145328,51
18^* * Central points.	20	65	50	106424019	3496468,34
19^* * Central points.	20	65	50	105421098	3797181,45

N°.	Classification	COVsa	Formula	CAS		SPME fibers
N°.	Classification	COVsa	Formula	CAS	PA	DVB/CAR/PDMS
1.		Sabinene hydrate	C₁₀H₁₈O	15537-55-0		X
2.		endo-Keto Borneol	C₁₀H₁₆O₂	114529-11-2	x
3.		6-Camphenol	C₁₀H₁₆O	55925-49-0		X
4.		cis-Crisantenol	C₁₀H₁₆O	55722-60-6		X
5.	Oxygenated monoterpenes	Dihydrocarbyl acetate	C₁₂H₂₀O₂	20777-49-5	x
6.		Eucalyptus	C₁₀H₁₈O	470-82-6		X
7.		cis-p-Mentha-2,8-dien-1-ol	C₁₀H₁₆O	22771-44-4		X
8.		Linalyl propionate	C₁₃H₂₂O₂	144-39-8	x
9.		α-campholenaldehyde	C₁₀H₁₆O	4501-58-0	x
10.		Carene	C₁₀H₁₆	13466-78-9	x	X
11.		Sylvestrene	C₁₀H₁₆	1461-27-4	x
12.	Monoterpene hydrocarbons	α-Fenchene	C₁₀H₁₆	7378-37-2	x
13.		α-Pinene¹ 1 Oliveira et al. (2018), (lyophilized fruits); '³ 3 Tietbohl et al. (2012), (leaves, stems and flowers); CAS: unique numerical identifier for chemical compounds	C₁₀H₁₆	2437-95-8	x	X
14.		β-Terpinene² 2 Ramos et al. (2010) (fresh leaves);	C₁₀H₁₆	99-84-3	x
15.		Agarospirol	C₁₅H₂₆O	23811-08-7	x
16.		Carotol	C₁₅H₂₆O	465-28-1	x
17.		Cubebol	C₁₅H₂₆O	23445-02-5	x	X
18.		Globulol² 2 Ramos et al. (2010) (fresh leaves);	C₁₅H₂₆O	489-41-8		X
19.	Oxygenated sesquiterpenes	Guaiol	C₁₅H₂₆O	489-86-1	x
20.		Terpinen-4-ol acetate	C₁₂H₂₀O₂	4821-04-9	x
21.		Viridiflorol	C₁₅H₂₄O^O	21747-46-6	x	X
22.		γ-Eudesmol² 2 Ramos et al. (2010) (fresh leaves);	C₁₅H₂₆O	1209-71-8	x
23.		Aromadendene	C₁₅H₂₄O	109119-91-7		X
24.		Allo-aromadendene² 2 Ramos et al. (2010) (fresh leaves);	C₁₅H₂₄O	25246-27-9		X
25.		Cadina-1 (10), 4-diene	C₁₅H₂₄O	16729-01-4	x
26.		Caryophyllene	C₁₅H₂₄O	13877-93-5	x	X
27.		Cyperene	C₁₅H₂₄O	2387-78-2	x
28.		Epizonarene	C₁₅H₂₄O	5975-30-4	x
29.		Germacrene D	C₁₅H₂₄O	37839-63-7		X
30.		Longifolene	C₁₅H₂₄O	475-20-7	x
31.		Patchoulene	C₁₅H₂₄O	1405-16-9	x
32.	Sesquiterpene hydrocarbons	Presilphiperfol-7-ene	C₁₅H₂₄O	80931-09-5	x
33.		Sativene	C₁₅H₂₄O	3650-28-0	x
34.		Valencene¹ 1 Oliveira et al. (2018), (lyophilized fruits);	C₁₅H₂₄O	4630-07-3	x
35.		α-Cubebene	C₁₅H₂₄O	17699-14-8	x	X
36.		α-Guaiene³ 3 Tietbohl et al. (2012), (leaves, stems and flowers); CAS: unique numerical identifier for chemical compounds	C₁₅H₂₄O	53863-54-0	x	X
37.		α-Gurjunene² 2 Ramos et al. (2010) (fresh leaves);	C₁₅H₂₄O	489-40-7		X
38.		α-Muurolene	C₁₅H₂₄O	10208-80-7		X
39.		α-Copaene	C₁₅H₂₄O	3856-25-5		X
40.		Calarene	C₁₅H₂₄O	17334-55-3	x
41.		β-Selinene¹ 1 Oliveira et al. (2018), (lyophilized fruits); '² 2 Ramos et al. (2010) (fresh leaves); '³ 3 Tietbohl et al. (2012), (leaves, stems and flowers); CAS: unique numerical identifier for chemical compounds	C₁₅H₂₄O	17066-67-0	x	X
42.		γ-Cadinene² 2 Ramos et al. (2010) (fresh leaves);	C₁₅H₂₄O	5957-55-1	x	X
43.		γ-Elemene	C₁₅H₂₄O	370572-92-2	x
44.		γ-Gurjunene	C₁₅H₂₄O	22567-17-5	x	X
45.		γ-Muurolene² 2 Ramos et al. (2010) (fresh leaves);	C₁₅H₂₄O	24268-39-1	x	X
46.		γ-Himachalene¹ 1 Oliveira et al. (2018), (lyophilized fruits);	C₁₅H₂₄O	53111-25-4	x	X
47.		δ -Cadinene² 2 Ramos et al. (2010) (fresh leaves);	C₁₅H₂₄O	483-76-1	x	X
48.		δ -Selinene	C₁₅H₂₄O	28624-23-9		X

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Optimization of extraction and identification of volatile compounds from Myrciaria floribunda1 1 Work extracted from the thesis of the first author, presented to the Graduate Program in Agronomy, Federal University of Alagoas/UFAL-AL

Otimização da extração e identificação dos compostos voláteis de Myrciaria floribunda

ABSTRACT

Optimization of extraction and identification of volatile compounds from Myrciaria floribunda¹ 1 Work extracted from the thesis of the first author, presented to the Graduate Program in Agronomy, Federal University of Alagoas/UFAL-AL