Microencapsulation of pequi pulp oil by complex coacervation

Pequi pulp oil, Caryocar brasiliense, is rich in carotenoids, antioxidant compound easily oxidized by the presence of heat, light and oxygen. In order to improve its stability, pequi oil was microencapsulated by complex coacervation using gelatin and Arabic gum as encapsulating agents. Twenty formulations were prepared using a 23 central composite rotational design. The influence of temperature, stirring velocity and core material in the oil coacervation were evaluated, aiming to preserve carotenoids present in the oil. The best yield values and carotenoids content were obtained at the midpoint of the design (7.5g core, 15.000rpm and 50°C). Particles showed asymmetric distribution, with diameter ranging from 15 to 145 µm and the efficiency of the encapsulation process, obtained by the retention of oil in the microcapsule, ranged from 66.58 to 96.50%, thus demonstrating the encapsulation efficiency of this method.

Index terms
Caryocar brasiliense; carotenoids; retention

Authorship

Priscilla Narciso Justi

Pharmacist, PhD, Universidade Federal do Mato Grosso do Sul. Dourados -MS. Email: priscillajusti@hotmail.com Universidade Federal de Mato Grosso do SulBrasilDourados, MS, Brasil Pharmacist, PhD, Universidade Federal do Mato Grosso do Sul. Dourados -MS. Email: priscillajusti@hotmail.com

Eliana Janet Sanjinez-Argandoña

Industrial Chemist, PhD, Universidade Federal do Grande Dourados. Dourados - MS. Email: elianaargandona@ufgd.edu.br Universidade Federal da Grande DouradosBrasilDourados, MS, Brasil Industrial Chemist, PhD, Universidade Federal do Grande Dourados. Dourados - MS. Email: elianaargandona@ufgd.edu.br

Maria Lígia Rodrigues Macedo

Biologist, PhD, Universidade Federal do Mato Grosso do Sul. Dourados - MS. Email: ligiamacedo18@gmail.com Universidade Federal de Mato Grosso do SulBrasilDourados, MS, Brasil Biologist, PhD, Universidade Federal do Mato Grosso do Sul. Dourados - MS. Email: ligiamacedo18@gmail.com

SCIMAGO INSTITUTIONS RANKINGS

Figures | Tables | Formulas

Figures (4)
Tables (5)
Formulas (7)

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Figure 1
Pareto plot, effects and interactions of temperature (° C), filling (g) and homogenization velocity (rpm) on the yield of pequi oil microcapsules.

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Figure 2
Graph of predicted and experimental values of the encapsulation efficiency of pequi oil. Efficiency p (%): efficiency values predicted by the mathematical model; Efficiency o (%): efficiency values experimentally obtained.

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Figure 3
Response surface (a) and contour graph (b) of velocity, temperature and filling interaction on the influence of carotenoid degradation on pequi pulp oil microcapsules.

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Figure 4
Particle size distribution.

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Table 1
Levels of independent variables used in the central composite rotational experimental design for the microencapsulation of pequi pulp oil.

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Table 2
Responses of the central composite rotational experimental design for pequi oil microcapsule using gum arabic and gelatin as encapsulants.

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Table 3
Regression parameters for the analysis of variance ANOVA of the microencapsulation yield of pequi oil (Caryocar brasiliense).

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Table 4
Regression parameters for the ANOVA analysis of variance of the efficiency of pequi oil microencapsulation (Caryocar brasiliense).

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Table 5
Regression parameters for the analysis of variance ANOVA of carotenoids from pequi oil microencapsulation (Caryocar brasiliense)

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Figure 1 Pareto plot, effects and interactions of temperature (° C), filling (g) and homogenization velocity (rpm) on the yield of pequi oil microcapsules.

Figure 2 Graph of predicted and experimental values of the encapsulation efficiency of pequi oil. Efficiency p (%): efficiency values predicted by the mathematical model; Efficiency o (%): efficiency values experimentally obtained.

Figure 3 Response surface (a) and contour graph (b) of velocity, temperature and filling interaction on the influence of carotenoid degradation on pequi pulp oil microcapsules.

Figure 4 Particle size distribution.

Table 1 Levels of independent variables used in the central composite rotational experimental design for the microencapsulation of pequi pulp oil.

Independent variables	Coded variables	Level
Independent variables	Coded variables	-1.68	-1	0	1	1.68
Temperature (°C)	X₁	33.2	40	50	60	66.8
Velocity (rpm)	X₂	6.600	10.000	15.000	20.000	23.400
Filling (g)	X₃	3.3	5	7.5	10	11.7

Table 2 Responses of the central composite rotational experimental design for pequi oil microcapsule using gum arabic and gelatin as encapsulants.

Test	A (ºC)	B (rpm)	C (g)	Yield (%)	Efficiency (%)	Carotenoids (µg/gms) *
1	40	10.000	5	67.07	66.58	60.30
2	40	10.000	10	79.12	78.06	40.95
3	40	20.000	5	73.91	74.68	46.86
4	40	20.000	10	76.70	75.64	29.27
5	60	10.000	5	72.45	71.80	31.84
6	60	10.000	10	80.29	79.96	49.32
7	60	20.000	5	71.65	71.99	25.83
8	60	20.000	10	77.06	76.26	24.96
9	33,2	15.000	7.5	74.75	75.20	25.25
10	66,8	15.000	7.5	72.30	72.42	24.73
11	50	6.600	7.5	77.70	76.83	23.95
12	50	23.400	7.5	75.67	76.25	21.74
13	50	15.000	3.3	73.01	74.28	44.15
14	50	15.000	11.7	79.49	79.06	23.85
15 (0)	50	15.000	7.5	96.76	96.24	192.15
16 (0)	50	15.000	7.5	97.07	96.86	191.60
17 (0)	50	15.000	7.5	96.40	96.70	191.48
18 (0)	50	15.000	7.5	96.91	96.34	191.96
19 (0)	50	15.000	7.5	96.45	96.68	192.10
20 (0)	50	15.000	7.5	96.67	96.50	192.04

^*
A, temperature (° C); B, homogenization velocity (rpm); C, filling (g); 0, central point *, expressed in dry mass.

Table 3 Regression parameters for the analysis of variance ANOVA of the microencapsulation yield of pequi oil (Caryocar brasiliense).

Factor	SQ	DF	QM	F	p
(1) Temperature (L)	0.042	1	0.042	0.048	0.828
Temperature (Q)	1876.699	1	1876.699	2132.520	≤0.05
(2) Velocity (L)	1.337	1	1.337	1.519	0.229
Velocity (Q)	1392.399	1	1392.399	1582.204	≤0.05
(3) Filling (L)	222.672	1	222.672	253.026	≤0.05
Filling ( (Q)	1455.460	1	1455.460	1653.860	≤0.05
1L 2L	17.808	1	17.808	20.236	≤0.05
1L 3L	0.624	1	0.624	0.709	0.407
2L 3L	34.164	1	34.164	38.821	≤0.05
Lack of adjustment	44.974	5	8.995	10.221	≤0.05
Pure error	22.001	25	0.880
Total SS	4297.590	39
R²	0.9844

^*
SQ, sum of squares; DF, degrees of freedom; QM, quadratic mean; F Fisher parameter for the significance test of effects; p (significance level =0.05).

Table 4 Regression parameters for the ANOVA analysis of variance of the efficiency of pequi oil microencapsulation (Caryocar brasiliense).

Factor	SQ	DF	QM	F	p
(1) Temperature (L)	0.020	1	0.020	0.031	0.862
Temperature (Q)	1864.557	1	1864.557	2917.342	≤0.05
(2) Velocity (L)	0.208	1	0.208	0.325	0.573
Velocity (Q)	1444.047	1	1444.047	2259.400	≤0.05
(3) Filling (L)	158.626	1	158.626	248.192	≤0.05
Filling (Q)	1424.986	1	1424.986	2229.576	≤0.05
1L 2L	21.045	1	21.045	32.928	≤0.05
1L 3L	0.000	1	0.000	0.000	0.997
2L 3L	51.876	1	51.876	81.167	≤0.05
Lack of adjustment	45.272	5	9.054	14.167	≤0.05
Pure error	15.978	25	0.639
Total SS	4253.893	39
R²	0.9856

Table 5 Regression parameters for the analysis of variance ANOVA of carotenoids from pequi oil microencapsulation (Caryocar brasiliense)

Factor	SQ	DF	QM	F	p
(1) Temperature (L)	314.2	1	314.19	806.3	≤0,05
Temperature (Q)	85430.0	1	85430.03	219238.5	≤0,05
(2) Velocity (L)	513.7	1	513.66	1318.2	≤0,05
Velocity (Q)	87827.9	1	87827.95	225392.3	≤0,05
(3) Filling (L)	434.2	1	434.23	1114.4	≤0,05
Filling (Q)	75720.1	1	75720.15	194320.1	≤0,05
1L 2L	6.9	1	6.88	17.6	≤0,05
1L 3L	716.5	1	716.50	1838.7	≤0,05
2L 3L	68.8	1	68.77	176.5	≤0,05
Lack of adjustment	3658.3	5	731.67	1877.7	≤0,05
Pure error	9.7	25	0.39
Total SS	213855.4	39
R²	0.9828

^*
SQ, sum of squares; DF, degrees of freedom; QM, quadratic mean; F Fisher parameter for the significance test of effects; p (significance level =0.05)

y = b_{0} + b_{1} x_{1} + b_{2} x_{2} + b_{3} x_{3} + b_{11} x_{1}^{2} + b_{22} x_{2}^{2} + b_{33} x_{3}^{2} + b_{12} x_{1} x_{2} + b_{13} x_{1} x_{3} + b_{23} x_{2} x_{3}

R (%) = \frac{{M S}_{b a s e s e c a}}{{M T I}_{b a s e s e c a}} \times 100

E (%) = \frac{O E M}{O I M} \times 100

C (\frac{μ g}{g}) = \frac{λ_{m a x} \times d \times 10^{4}}{ε \times m}

R (%) = - 272,11 + 8,46 \times A - 0,08 \times A^{2} + 0,01 \times B - 2,8 \times 10^{- 7} \times B^{2} - 2,1 \times 10^{- 5} \times A \times B - 7,9 \times 10^{- 3} \times 7,5 \times A - 1,2 \times 10^{- 4} \times 7,5 \times B + 88,74

E = - 205,35 + 6,79 \times A - 0,08 \times A^{2} + 0,01 \times B - 2,8 \times 10^{- 7} \times B^{2} - 2,3 \times 10^{- 5} \times 7,5 \times A - 1,4 \times 10^{- 4} \times 7,5 \times B + 86,83

C a r = - 2025,74 + 52,57 \times A - 0,54 \times A^{2} + 0,068 \times B - 2,2 \times 10^{- 6} - 1,3 \times 10^{- 5} \times A \times B + 0,27 \times 7,5 \times A - 1,6 \times 10^{- 4} \times B + 370,1

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Este documento possui uma errata:

10.1590/0100-29452018874erratum

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Microencapsulation of pequi pulp oil by complex coacervation

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[TFN0201] ^*
A, temperature (° C); B, homogenization velocity (rpm); C, filling (g); 0, central point *, expressed in dry mass.