CHEMOMETRIC STRATEGY FOR OPTIMIZATION OF AN ACID DECOMPOSITION METHOD TO DETERMINE THE MINERAL COMPOSITION IN ALMOND PULP (<i>Terminalia catappa</i> Linn.)

Santos, Ana Maria Pinto dos; Santos, Liz Oliveira dos; Santos, Lorena de Souza; Silva, Emmanuelle Ferreira Requião; Neto, João Honorato Santos; Brandão, Geovani Cardoso

doi:10.21577/0100-4042.20170732

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Artigo • Sociedade Brasileira de Química 44 (7) • 2021 • https://doi.org/10.21577/0100-4042.20170732 copy

CHEMOMETRIC STRATEGY FOR OPTIMIZATION OF AN ACID DECOMPOSITION METHOD TO DETERMINE THE MINERAL COMPOSITION IN ALMOND PULP (Terminalia catappa Linn.)

Authorship SCIMAGO INSTITUTIONS RANKINGS

In this work, multivariate optimization techniques were applied to develop an acid digestion procedure in digester block using “cold finger” as reflux system to determine minerals in almond pulp samples by inductively coupled plasma optical emission spectrometry. Two-level full factorial design and Box-Behnken design were applied to evaluate and optimize the factors involved in the acid digestion process. In both experimental designs, Function D and Function MR multiple responses were used to establish the method condition for all analytes and with greater digestion efficiency. Two apple and spinach leaves certified reference materials were analyzed to confirm the proposed method accuracy. The digestion efficiency was evaluated by residual carbon content which showed 1.32-1.77% range. The concentration values found for each element in almond pulp collected in Salvador, Bahia, Brazil in mg 100 g^-1; were: 3.08 (Ca), 0.209 (Cu), 0.407 (Fe), 356 (K), 21.5 (Mg), 0.096 (Mn), 34.4 (P) and 0.289 (Zn). The developed method was simple and efficient for almond pulp mineral composition evaluation. This unconventional fruit has nutritional relevance with future application for new food recipes and pharmaceutical products formulation.

Keywords:
almonds; mineral composition; Box-Behnken design; desirability function; MR function

Experiment	Volume (mL)			MR	D
Experiment	HNO₃	H₂SO₄	H₂O₂	MR	D
1	−1 (1.5)	−1 (0.5)	−1 (0.2)	7.966	0.992
2	−1 (1.5)	−1 (0.5)	1 (0.8)	7.837	0.958
3	−1 (1.5)	1 (1.5)	−1 (0.2)	5.182	0.248
4	−1 (1.5)	1 (1.5)	1 (0.8)	4.919	0.182
5	1 (2.5)	−1 (0.5)	−1 (0.2)	7.339	0.827
6	1 (2.5)	−1 (0.5)	1 (0.8)	7.054	0.752
7	1 (2.5)	1 (1.5)	−1 (0.2)	6.699	0.655
8	1 (2.5)	1 (1.5)	1 (0.8)	4.201	0.000
9	0 (2.0)	0 (1.0)	0 (0.5)	5.430	0.324
10	0 (2.0)	0 (1.0)	0 (0.5)	5.617	0.369
11	0 (2.0)	0 (1.0)	0 (0.5)	5.663	0.387

Term	Regression coefficients
Term	MR	D
Independent	12.141	2.102
*NV^ * Significant: MR = Multiple Response; D = Desirability; NV = Nitric acid volume; SV = Sulfuric acid volume; PV = Hydrogen peroxide volume.**	-1.993	-0.528
*SV^ * Significant: MR = Multiple Response; D = Desirability; NV = Nitric acid volume; SV = Sulfuric acid volume; PV = Hydrogen peroxide volume.**	-6.995	-1.864
PV	-2.312	-0.607
NV by *SV^ * Significant: MR = Multiple Response; D = Desirability; NV = Nitric acid volume; SV = Sulfuric acid volume; PV = Hydrogen peroxide volume.**	2.837	0.754
NV by PV	1.473	0.386
SV by PV	4.976	1.312
NV by SV by *PV^ * Significant: MR = Multiple Response; D = Desirability; NV = Nitric acid volume; SV = Sulfuric acid volume; PV = Hydrogen peroxide volume.**	-3.466	-0.912

Factor	Multiple Response (MR)		Desirability (D)
Factor	F	p	F	p
NV	3.056	0.222	2.562	0.251
SV^* * Significant: NV = Nitric acid volume; SV = Sulfuric acid volume; PV = Hydrogen peroxide volume.	693.149	0.001	715.968	0.001
PV^* * Significant: NV = Nitric acid volume; SV = Sulfuric acid volume; PV = Hydrogen peroxide volume.	82.632	0.012	82.609	0.012
NV by SV^* * Significant: NV = Nitric acid volume; SV = Sulfuric acid volume; PV = Hydrogen peroxide volume.	39.952	0.024	42.775	0.023
NV by PV^* * Significant: NV = Nitric acid volume; SV = Sulfuric acid volume; PV = Hydrogen peroxide volume.	46.902	0.021	47.669	0.020
SV by PV^* * Significant: NV = Nitric acid volume; SV = Sulfuric acid volume; PV = Hydrogen peroxide volume.	45.170	0.021	45.172	0.021
NV by SV by PV^* * Significant: NV = Nitric acid volume; SV = Sulfuric acid volume; PV = Hydrogen peroxide volume.	35.454	0.027	35.898	0.027
Lack of Fit^* * Significant: NV = Nitric acid volume; SV = Sulfuric acid volume; PV = Hydrogen peroxide volume.	98.490	0.010	97.975	0.010

Factor	Multiple Response (MR)			Desirability (D)
Factor	Effect	t(2)	p	Effect	t(2)	p
NV	-0.153	-1.748	0.222	-0.037	-1.601	0.251
SV^* Significant: MR = Multiple response; D = Desirability function.	-2.299	-26.328	0.001	-0.611	-26.758	0.001
PV^* Significant: MR = Multiple response; D = Desirability function.	-0.794	-9.090	0.012	-0.207	-9.089	0.012
NV by SV^* Significant: MR = Multiple response; D = Desirability function.	0.552	6.321	0.024	0.149	6.540	0.023
NV by PV^* * Significant: NV = Nitric acid volume; SV = Sulfuric acid volume; PV = Hydrogen peroxide volume.	-0.598	-6.848	0.021	-0.158	-6.904	0.020
SV by PV^* Significant: MR = Multiple response; D = Desirability function.	-0.587	-6.721	0.021	-0.153	-6.721	0.021
NV by SV by PV*	-0.520	-5.954	0.027	-0.137	-5.992	0.027

Experiment	Volume (mL)			MR	D
Experiment	HNO₃	H₂SO₄	H₂O₂	MR	D
1	-1 (1.5)	−1 (0.2)	0 (0.5)	6.422	0.682
2	1 (2.5)	−1 (0.2)	0 (0.5)	4.253	0.242
3	−1 (1.5)	1 (1.0)	0 (0.5)	3.914	0.190
4	1 (2.5)	1 (1.0)	0 (0.5)	2.866	0.000
5	-1 (1.5)	0 (0.6)	−1 (0.2)	5.492	0.499
6	1 (2.5)	0 (0.6)	−1 (0.2)	3.881	0.191
7	−1 (1.5)	0 (0.6)	1 (0.8)	7.194	0.830
8	1 (2.5)	0 (0.6)	1 (0.8)	6.530	0.710
9	0 (2.0)	−1 (0.2)	−1 (0.2)	7.193	0.817
10	0 (2.0)	1 (1.0)	−1 (0.2)	3.363	0.084
11	0 (2.0)	−1 (0.2)	1 (0.8)	6.862	0.758
12	0 (2.0)	1 (1.0)	1 (0.8)	6.338	0.655
13	0 (2.0)	0 (0.6)	0 (0.5)	6.166	0.624
14	0 (2.0)	0 (0.6)	0 (0.5)	6.491	0.676
15	0 (2.0)	0 (0.6)	0 (0.5)	6.326	0.620

Factor	Multiple Response (MR)		Desirability (D)
Factor	F	p	F	p
(1)NV(L)^* * Significant: NV = Nitric acid volume; SV = Sulfuric acid volume; PV = Hydrogen peroxide volume.	143.115	0.007	143.995	0.007
NV(Q)^* * Significant: NV = Nitric acid volume; SV = Sulfuric acid volume; PV = Hydrogen peroxide volume.	158.831	0.006	138.653	0.007
(2)SV(L)^* * Significant: NV = Nitric acid volume; SV = Sulfuric acid volume; PV = Hydrogen peroxide volume.	322.742	0.003	317.194	0.003
SV(Q)^* * Significant: NV = Nitric acid volume; SV = Sulfuric acid volume; PV = Hydrogen peroxide volume.	113.303	0.009	109.735	0.009
(3)PV(L)^* * Significant: NV = Nitric acid volume; SV = Sulfuric acid volume; PV = Hydrogen peroxide volume.	232.077	0.004	238.297	0.004
PV(Q)^* * Significant: NV = Nitric acid volume; SV = Sulfuric acid volume; PV = Hydrogen peroxide volume.	36.532	0.026	44.670	0.022
NV (L) by SV (L)	11.939	0.075	16.047	0.057
NV (L) by PV (L)	8.510	0.100	9.090	0.095
SV (L) by PV (L)^* * Significant: NV = Nitric acid volume; SV = Sulfuric acid volume; PV = Hydrogen peroxide volume.	103.717	0.010	102.298	0.010
Lack of Fit	6.348	0.139	7.081	0.126

Factor	Multiple Response (MR)			Desirability (D)
Factor	Effect	t(2)	p	Effect	t(2)	p
(1)NV(L)^* * Significant: NV = Nitric acid volume; SV = Sulfuric acid volume; PV = Hydrogen peroxide volume.	-1.373	-11.963	0.007	-0.265	-12.000	0.007
NV(Q)^* * Significant: NV = Nitric acid volume; SV = Sulfuric acid volume; PV = Hydrogen peroxide volume.	1.065	12.603	0.006	0.191	11.775	0.007
(2)SV(L)^* * Significant: NV = Nitric acid volume; SV = Sulfuric acid volume; PV = Hydrogen peroxide volume.	-2.062	-17.965	0.003	-0.393	-17.810	0.003
SV(Q)^* * Significant: NV = Nitric acid volume; SV = Sulfuric acid volume; PV = Hydrogen peroxide volume.	0.899	10.644	0.009	0.170	10.475	0.009
(3)PV(L)^* * Significant: NV = Nitric acid volume; SV = Sulfuric acid volume; PV = Hydrogen peroxide volume.	1.749	15.234	0.004	0.341	15.437	0.004
PV(Q)^* * Significant: NV = Nitric acid volume; SV = Sulfuric acid volume; PV = Hydrogen peroxide volume.	-0.511	-6.044	0.026	-0.109	-6.684	0.022
NV (L) by SV (L)	0.561	3.455	0.075	0.125	4.006	0.057
NV (L) by PV (L)	0.474	2.917	0.100	0.094	3.015	0.095
SV (L) by PV (L)^* * Significant: NV = Nitric acid volume; SV = Sulfuric acid volume; PV = Hydrogen peroxide volume.	1.653	10.184	0.010	0.316	10.114	0.010

Factor	Observed minimum	Critical value (RM)	Critical value (D)	Observed maximum
NV	1.500	1.782	1.758	2.500
SV	0.200	0.312	0.306	1.000
VP	0.200	0.448	0.456	0.800

Element	LOD (mg kg^-1;)	LOQ (mg kg^-1;)	Found value (mg kg^-1;)	Certified value (mg kg^-1;)	t-calculated value
Ca	6.0	19.9	14681 ± 836	15250 ± 100^a	2.93
Cu	0.15	0.49	10.42 ± 1.77	12.22 ± 0.86^b	4.25
Fe	1.0	3.4	85.7 ± 3.7	82.7 ± 2.6^a	3.49
K	2.8	9.2	15447 ± 1054	16080 ± 210^a	2.58
Mg	0.77	2.58	2480 ± 222	2710 ± 120^a	4.07
Mn	0.10	0.33	55.3 ± 2.8	54.1 ± 1.1^a	1.84
P	1.4	4.6	1529 ± 168	1593 ± 68^a	1.64
Zn	0.43	1.44	11.80 ± 1.20	12.45 ± 0.43^a	2.33

Element	Mineral composition (mg 100 g^-1;)
Element	Almond^a aThis work. The results for almond mineral composition were expressed as wet basis. bSantos et al.37cTACO.38dUSDA.39eUdotong et al.40 Almonds of the species Terminalia catappa L.fYada et al.41 Almonds of the species Prunus dulcis.	Atemoya^b aThis work. The results for almond mineral composition were expressed as wet basis. bSantos et al.37cTACO.38dUSDA.39eUdotong et al.40 Almonds of the species Terminalia catappa L.fYada et al.41 Almonds of the species Prunus dulcis.	Avocado^c aThis work. The results for almond mineral composition were expressed as wet basis. bSantos et al.37cTACO.38dUSDA.39eUdotong et al.40 Almonds of the species Terminalia catappa L.fYada et al.41 Almonds of the species Prunus dulcis.	Melon^d aThis work. The results for almond mineral composition were expressed as wet basis. bSantos et al.37cTACO.38dUSDA.39eUdotong et al.40 Almonds of the species Terminalia catappa L.fYada et al.41 Almonds of the species Prunus dulcis.	Papaya^d aThis work. The results for almond mineral composition were expressed as wet basis. bSantos et al.37cTACO.38dUSDA.39eUdotong et al.40 Almonds of the species Terminalia catappa L.fYada et al.41 Almonds of the species Prunus dulcis.	Watermeloⁿ aThis work. The results for almond mineral composition were expressed as wet basis. bSantos et al.37cTACO.38dUSDA.39eUdotong et al.40 Almonds of the species Terminalia catappa L.fYada et al.41 Almonds of the species Prunus dulcis. d	Almond^e aThis work. The results for almond mineral composition were expressed as wet basis. bSantos et al.37cTACO.38dUSDA.39eUdotong et al.40 Almonds of the species Terminalia catappa L.fYada et al.41 Almonds of the species Prunus dulcis.	Almond^f aThis work. The results for almond mineral composition were expressed as wet basis. bSantos et al.37cTACO.38dUSDA.39eUdotong et al.40 Almonds of the species Terminalia catappa L.fYada et al.41 Almonds of the species Prunus dulcis.
Ca	3.08	11.8	0.13	6	11.1	7	1.19	430
Cu	0.209	0.150	-	0.024	0.025	0.042	-	1.1
Fe	0.407	0.750	0.61	0.17	0.25	0.240	0.001	3.5
K	356	1362	504	228	146	112	2	685
Mg	21.5	64.4	29	10	11.1	10	1.3	420
Mn	0.096	0.350	-	0.027	-	0.038	-	1.5
Na	2.12	13.3	8	18	1.98	1	1.95	10.5
P	34.4	47.5	54	11	5.36	110	22.6	705
Zn	0.289	0.930	0.68	0.09	0.03	0.100	0.163	3.55

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