USE OF MIP OES AND F AAS/AES FOR DETERMINATION OF Ca, K, Na AND Mg IN BRAZILIAN CREAM CHEESE

Diniz, Leila M. N.; Carrasco, Thaiane S.; Medina, Aline L.; Ribeiro, Anderson S.; Nunes, Adriane M.

doi:10.21577/0100-4042.20170049

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Artigo • Quím. Nova 40 (7) • Aug 2017 • https://doi.org/10.21577/0100-4042.20170049 copy

USE OF MIP OES AND F AAS/AES FOR DETERMINATION OF Ca, K, Na AND Mg IN BRAZILIAN CREAM CHEESE

Authorship SCIMAGO INSTITUTIONS RANKINGS

In this work, two sample preparation procedures for subsequent determination of Na, K, Ca and Mg by techniques of atomic spectrometry in samples of Brazilian cream cheese were evaluated. The determinations were performed on two equipments, F AAS and MIP OES, which presented similar results, being evident the advantages of MIP OES since it is a multielementar technique with low operational cost and high efficiency. The first procedure was carried out by acidic decomposition (HNO₃/H₂SO₄) in a reflux system, and the second used the alkaline solubilization with tetramethylammonium hydroxide. The accuracy was verified by recovery tests and the results were between 80 and 104% for both procedures. A comparison with a reference procedure was also performed and no significant differences have been observed at the 95% confidence level. The evaluated elements were not in accordance with the values indicated on the labels of all products, showing the importance for monitoring these products. The methods of sample preparation proposed showed to be simple, inexpensive, providing accurate and precise results, and are a promising alternative to be used for the quality control of these routine test samples.

Keywords:
Brazilian cream cheese; acid decomposition; alkaline solubilization; F AAS; MIP OES

Parameters	Analyte
Parameters	Na	K	Ca	Mg
	F AAS/AES
Wavelength (nm)	589.00	766.49	422.67	285.21
Lamp current (mA)	-	-	10	6
Spectral band pass (mm)	1.8	2.7	2.7	2.7
	MIP OES
Wavelength (nm)	588.995	766.491	393.366	285.995
Viewing position	0	10	10	0
Nebulizer flow (L/min)	1	1	0.65	0.8

Runs	Independent variables				Analytical signals
Runs	Sample mass (mg)	H₂SO₄volume (mL)	Time (h)	Temperature (°C)	Na^* * Emission signal;	K^* * Emission signal;	Ca^ Absorbance signal.	Mg^ Absorbance signal.
1	625	1.5	1.5	295	2071667	165175	0.579	1.108
2	875	1.5	1.5	295	2626467	233590	0.710	1.282
3	625	2.5	1.5	295	2097800	164985	0.645	1.047
4	875	2.5	1.5	295	2725867	234060	0.692	1.263
5	625	1.5	2.5	295	2070067	169275	0.721	1.083
6	875	1.5	2.5	295	2607333	235405	0.699	1.271
7	625	2.5	2.5	295	2068867	166415	0.629	1.067
8	875	2.5	2.5	295	2549067	230155	0.693	1.269
9	625	1.5	1.5	325	2055133	173995	0.638	1.069
10	875	1.5	1.5	325	2595667	240030	0.678	1.286
11	625	2.5	1.5	325	1893800	172175	0.648	1.076
12	875	2.5	1.5	325	2350000	235395	0.689	1.275
13	625	1.5	2.5	325	2043533	170880	0.727	1.094
14	875	1.5	2.5	325	2515733	236395	0.708	1.307
15	625	2.5	2.5	325	2025733	175680	0.632	1.060
16	875	2.5	2.5	325	2612067	236945	0.702	1.282
17	500	2.0	2.0	310	1624133	132710	0.591	0.954
18	1000	2.0	2.0	310	3043533	262250	0.756	1.357
19	750	1.0	2.0	310	2295200	194975	0.687	1.208
20	750	3.0	2.0	310	2715000	208520	0.658	1.222
21	750	2.0	1.0	310	2440800	203325	0.611	1.191
22	750	2.0	3.0	310	2304800	197077	0.766	1.224
23	750	2.0	2.0	280	2173133	203085	0.609	1.171
24	750	2.0	2.0	340	2090933	207760	0.792	1.187
25	750	2.0	2.0	310	2403200	211215	0.654	1.211
26	750	2.0	2.0	310	2389300	203895	0.659	1.211
27	750	2.0	2.0	310	2342000	200145	0.613	1.206

Runs	Independent variables		Analytical signals
Runs	Sample mass (mg)	TMAH volume (µL)	Na^* * Emission signal;	K^* * Emission signal;	Ca^ Absorbance signal.	Mg^ Absorbance signal.
1	85	160	291909.667	455442.000	0.160	0.196
2	265	160	457286.667	830612.000	0.368	0.360
3	85	440	304107.333	459740.667	0.131	0.190
4	265	440	470893.000	859429.000	0.314	0.353
5	50	300	245049.333	359873.667	0.100	0.162
6	300	300	488353.000	8989913.667	0.337	0.369
7	175	100	404649.000	702303.333	0.247	0.283
8	175	500	407580.000	697333.667	0.212	0.281
9	175	300	406746.667	703159.333	0.212	0.270
10	175	300	405201.333	677741.334	0.193	0.257
11	175	300	407749.000	689217.333	0.191	0.259

	Acid decomposition			Solubilization with TMAH
	Added value (mg g^-1)	Found value* (mg g^-1)	Recovery (%)	Added value (mg g^-1)	Found value* (mg g^-1)	Recovery (%)
Na	0.00	7.39 ± 0.29	-	0.00	7.18 ± 0.08	-
	3.43	10.60 ± 0.19	94	2.50	9.78 ± 0.06	104
	9.14	15.92 ± 0.16	93	6.67	13.29 ± 0.11	92
	17.13	21.24 ± 0.35	81	10.00	16.15 ± 0.09	90
K	0.00	0.76 ± 0.01	-	0.00	0.75 ± 0.03	-
	0.46	1.15 ± 0.01	85	0.75	1.49 ± 0.04	99
	0.86	1.50 ± 0.01	86	2.00	2.82 ± 0.06	104
	1.37	1.86 ± 0.01	80	3.67	3.69 ± 0.02	80
Ca	0.00	2.22 ± 0.07	-	0.00	1.98 ± 0.01	-
	1.71	3.84 ± 0.03	95	5.00	6.68 ± 0.03	94
	3.08	4.84 ± 0.16	85	8.30	9.08 ± 0.01	86
	4.28	5.68 ± 0.03	81	11.70	13.88 ± 0.08	102
Mg	0.00	0.108 ± 0.002	-	0.00	0.11 ± 0.01	-
	0.19	0.304 ± 0.003	103	0.13	0.24 ± 0.01	100
	0.32	0.427 ± 0.005	100	0.21	0.320 ± 0.01	100
	0.43	0.540 ± 0.013	100	0.29	0.40 ± 0.01	100

Analyte	Procedure	Concentration (mg g^-1) ± SD	RSD %
Na	1	7.35 ± 0.15	2.04
	2	7.00 ± 0.15	2.14
	3	8.00 ± 0.03	0.38
K	1	0.76 ± 0.01	1.32
	2	0.75 ± 0.02	2.67
	3	0.80 ± 0.01	1.25
Ca	1	2.23 ± 0.01	0.45
	2	1.98 ± 0.05	2.53
	3	2.03 ± 0.13	6.40
Mg	1	0.108 ± 0.002	1.85
	2	0.110 ± 0.002	1.82
	3	0.107 ± 0.004	3.74

Analyte	Analytical technique	Procedure	Range (mgL^-1)	a (L mg^-1)	R	LOD^* * equipment limit of detection; (mg L^-1)	LOD^ method limit of detection. (µg g^-1)
Na	F AES	1	0.25 - 1.5	14703.49	0.991	0.01	0.43
	F AES	2	0.25 - 1.5	16063.86	0.992	0.002	0.81
	MIP OES	1	0.25 - 1.5	672308.67	0.999	0.01	0.27
	MIP OES	2	0.25 - 1.5	668683.26	0.999	0.003	0.24
K	F AES	1	0.25 - 1.5	14567.46	0.999	0.003	0.36
	F AES	2	0.25 - 1.5	15122.71	0.999	0.003	0.74
	MIP OES	1	0.25 - 1.5	138374.93	0.999	0.002	0.08
	MIP OES	2	0.25 - 1.5	115606.64	0.998	0.003	0.29
Ca	F AAS	1	1.0 - 4.0	0.06	0.991	0.02	2.69
	F AAS	2	1.0 - 4.0	0.06	0.999	0.03	33.07
	MIP OES	1	1.0 - 4.0	532036.32	0.998	0.01	0.23
	MIP OES	2	1.0 - 4.0	552129.78	0.999	0.01	0.27
Mg	F AAS	1	0.1 - 0.4	0.97	0.999	0.003	0.18
	F AAS	2	0.1 - 0.4	0.90	0.999	0.003	0.83
	MIP OES	1	0.1 - 0.4	380869.89	0.997	0.001	0.03
	MIP OES	2	0.1 - 0.4	353678.66	0.998	0.003	0.06

Analyte	Analytical technique	Procedure	Samples
Analyte	Analytical technique	Procedure	Sample 2	Sample 3	Sample 4	Sample 5	Sample 6
Na	F AES	1	6.30 ± 0.34	6.97 ± 0.58	5.82 ± 0.46	7.77 ± 0.11	6.76 ± 0.26
	F AES	2	6.85 ± 0.16	7.23 ± 0.04	6.20 ± 0.06	7.82 ± 0.15	6.81 ± 0.04
	MIP OES	1	5.28 ± 0.07	5.84 ± 0.02	4.98 ± 0.09	5.51 ± 0.05	5.13 ± 0.04
	MIP OES	2	6.42 ± 0.13	7.07 ± 0.09	5.30 ± 0.02	6.07 ± 0.06	5.22 ± 0.01
K	F AES	1	0.84 ± 0.01	0.31 ± 0.01	0.858 ± 0.001	1.07 ± 0.04	4.61 ± 0.07
	F AES	2	0.83 ± 0.01	0.289 ± 0.002	0.85 ± 0.01	1.096 ± 0.004	4.48 ± 0.03
	MIP OES	1	0.65 ± 0.02	0.30 ± 0.01	0.86 ± 0.02	1.02 ± 0.01	4.50 ± 0.1
	MIP OES	2	0.84 ± 0.01	0.35 ± 0.02	0.89 ± 0.02	1.08 ± 0.03	4.48 ± 0.04
Ca	F AAS	1	2.15 ± 0.01	3.39 ± 0.10	3.23 ± 0.09	3.69 ± 0.03	3.26 ± 0.02
	F AAS	2	2.129 ± 0.004	3.03 ± 0.12	3.13 ± 0.01	3.61 ± 0.03	3.24 ± 0.02
	MIP OES	1	2.16 ± 0.02	2.87 ± 0.03	3.07 ± 0.14	3.71 ± 0.09	3.71 ± 0.09
	MIP OES	2	2.10 ± 0.1	3.15 ± 0.02	3.27 ± 0.05	3.58 ± 0.06	3.58 ± 0.06
Mg	F AAS	1	0.10 ± 0.01	0.101 ± 0.002	0.167 ± 0.002	0.226 ± 0.002	0.228 ± 0.004
	F AAS	2	0.107 ± 0.001	0.107 ± 0.001	0.17 ± 0.01	0.224 ± 0.002	0.229 ± 0.002
	MIP OES	1	0.10 ± 0.01	0.101 ± 0.003	0.16 ± 0.01	0.214 ± 0.007	0.22 ± 0.01
	MIP OES	2	0.105 ± 0.001	0.099 ± 0.004	0.17 ± 0.01	0.23 ± 0.01	0.22 ± 0.01

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