Application of Factorial Design and Desirability Function to Develop a Single Analytical Procedure for the Determination of Metals in Different Tissues of Blue Crab (Callinectes danae)

Lima, Daniel C.; Guedes, Wesley N.; Costa, Vinicius C.; Amorim, Fábio A. C.

doi:10.21577/0103-5053.20180064

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Journal of the Brazilian Chemical Society

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Articles • J. Braz. Chem. Soc. 29 (9) • Sept 2018 • https://doi.org/10.21577/0103-5053.20180064 copy

Application of Factorial Design and Desirability Function to Develop a Single Analytical Procedure for the Determination of Metals in Different Tissues of Blue Crab (Callinectes danae)

Authorship SCIMAGO INSTITUTIONS RANKINGS

In this scientific work, it was developed a single analytical procedure for the sample preparation of different tissues of blue crabs using microwave-assisted digestion for the determination of Cu, Mn, Fe and Zn by fast sequential flame atomic absorption spectrometry (FS FAAS). The limits of quatification were 10.5, 1.6, 8.9 and 19.3 µg g^-1 for Cu, Mn, Fe and Zn, respectively. The precision was estimated in terms of repeatability using the relative standard deviation (RSD, n = 7) 3.4% for Cu; 4.8% (Mn); 4.7% (Fe) and 4.7% (Zn) and accuracy of the procedure was confirmed by analysis of certified reference material (CRM) of oyster tissue (NIST 1566B) with concentration values of 71.3 for Cu, 18.3 for Mn, 202.5 for Fe and 1415 µg g^-1 for Zn. The procedure has been applied for the determination of Cu, Mn, Fe and Zn in several blue crab samples from Cachoeira River estuary, Ilhéus, Bahia, Brazil.

Keywords:
factorial design; desirability function; effect of matrix; singles analytical procedure

Experiment	Temperature / °C	time / min	HNO₃ / mL	H₂O₂ / mL	OD legs	OD hepato
1	120 (–1)	15 (–1)	1 (–1)	1 (–1)	0.00	0.63
2	160 (+1)	15 (–1)	1 (–1)	1 (–1)	0.75	0.00
3	120 (–1)	21 (+1)	1 (–1)	1 (–1)	0.69	0.00
4	160 (+1)	21 (+1)	1 (–1)	1 (–1)	0.69	0.73
5	120 (–1)	15 (–1)	3 (+1)	1 (–1)	0.00	0.58
6	160 (+1)	15 (–1)	3 (+1)	1 (–1)	0.74	0.56
7	120 (–1)	21 (+1)	3 (+1)	1 (–1)	0.73	0.60
8	160 (+1)	21 (+1)	3 (+1)	1 (–1)	0.73	0.74
9	120 (–1)	15 (–1)	1 (–1)	3 (+1)	0.00	0.57
10	160 (+1)	15 (–1)	1 (–1)	3 (+1)	0.72	0.69
11	120 (–1)	21 (+1)	1 (–1)	3 (+1)	0.75	0.78
12	160 (+1)	21 (+1)	1 (–1)	3 (+1)	0.75	0.73
13	120 (–1)	15 (–1)	3 (+1)	3 (+1)	0.00	0.61
14	160 (+1)	15 (–1)	3 (+1)	3 (+1)	0.70	0.78
15	120 (–1)	21 (+1)	3 (+1)	3 (+1)	0.79	0.71
16	160 (+1)	21 (+1)	3 (+1)	3 (+1)	0.77	0.72
17	140 (0)	18 (0)	2 (0)	2 (0)	0.74	0.67
18	140 (0)	18 (0)	2 (0)	2 (0)	0.71	0.66
19	140 (0)	18 (0)	2 (0)	2 (0)	0.71	0.67

Analyte	Mean	Calibration technique	Equation	r²
Cu	aqueous	conventional	y = (0.1020 ± 0.0018)C_Cu + (0.0028 ± 0.0037)	0.9998
	acidic	residual acidity	y = (0.1007 ± 0.0014)C_Cu + (0.0037 ± 0.0028)	0.9999
	hepato^a a Hepato: hepatopancreas;	st. add. techn.	y = (0.1002 ± 0.0015)C_Cu + (0.0647 ± 0.0032)	0.9998
	claws^b b claws muscles;	st. add. techn.	y = (0.1026 ± 0.0024)C_Cu + (0.0223 ± 0.0050)	0.9996
	legs^c c legs: legs muscles; r2: coefficient of determination; st. add. techn.: standard addition technique.	st. add. techn.	y = (0.1000 ± 0.0015)C_Cu + (0.0303 ± 0.0030)	0.9998
Mn	aqueous	conventional	y = (0.1517 ± 0.0035)C_Mn + (0.0026 ± 0.0041)	0.9996
	acidic	residual acidity	y = (0.1528 ± 0.0034)C_Mn + (0.0020 ± 0.0039)	0.9996
	hepato	st. add. techn.	y = (0.1526 ± 0.0029)C_Mn + (0.0343 ± 0.0034)	0.9997
	claws	st. add. techn.	y = (0.1516 ± 0.0026)C_Mn + (0.0033 ± 0.0030)	0.9998
	legs	st. add. techn.	y = (0.1536 ± 0.0032)C_Mn + (0.0028 ± 0.0037)	0.9997
Fe	aqueous	conventional	y = (0.0513 ± 0.0007)C_Fe + (0.0095 ± 0.0015)	0.9999
	acidic	residual acidity	y = (0.0507 ± 0.0017)C_Fe + (0.0055 ± 0.0035)	0.9992
	hepato	st. add. techn.	y = (0.0517 ± 0.0019)C_Fe + (0.0139 ± 0.0039)	0.9990
	claws	st. add. techn.	y = (0.0515 ± 0.0019)C_Fe + (0.0089 ± 0.0039)	0.9990
	legs	st. add. techn.	y = (0.0513 ± 0.0013)C_Fe + (0.0062 ± 0.0026)	0.9995
Zn	aqueous	conventional	y = (0.2126 ± 0.0056)C_Zn + (0.0042 ± 0.0034)	0.9995
	acidic	residual acidity	y = (0.2086 ± 0.0056)C_Zn + (0.0076 ± 0.0035)	0.9994
	hepato	st. add. techn.	y = (0.2124 ± 0.0074)C_Zn + (0.0370 ± 0.0046)	0.9991
	claws	st. add. techn.	y = (0.2041 ± 0.0067)C_Zn + (0.0383 ± 0.0041)	0.9992
	legs	st. add. techn.	y = (0.2044 ± 0.0055)C_Zn + (0.0401 ± 0.0034)	0.9994

Analyte	Concentration / (µg g^-1)		Test CRM (expanded uncertainty)
Analyte	Certified value	Proposed procedure	Test CRM (expanded uncertainty)
Cu	71.6 ± 1.6	71.3 ± 2.3	0.3 ≤ 2.89
Mn	18.5 ± 0.2	18.3 ± 0.9	0.2 ≤ 1.13
Fe	205.8 ± 6.8	202.5 ± 2.5	1.4 ≤ 5.19
Zn	1424 ± 46	1415 ± 36	9.0 ≤ 51.04

Sample	Point 1 (n = 12 animals)				Point 2 (n = 25 animals)				Point 3 (n = 10 animals)
	Concentration / (µg g^-1)				Concentration / (µg g^-1)				Concentration / (µg g^-1)
	Cu	Mn	Fe	Zn	Cu	Mn	Fe	Zn	Cu	Mn	Fe	Zn
Claws muscles (7 replicates)	47.8	2.49	18.1	940	56.7	4.53	10.7	956	39.0	2.04	14.0	913
	50.9	2.71	16.2	925	57.5	4.58	10.1	963	38.9	1.97	14.4	903
	50.5	2.41	16.7	926	58.7	4.44	10.7	975	37.3	2.04	13.8	896
	49.4	2.21	17.9	946	59.3	4.10	10.8	979	36.6	2.02	12.9	923
	48.4	2.59	16.2	941	54.5	4.03	11.9	993	37.5	1.95	12.9	917
	50.6	2.10	16.2	949	55.1	4.12	10.4	995	37.0	2.05	14.3	940
	50.5	2.54	16.2	954	55.0	4.49	10.0	957	41.6	2.22	13.9	933
Legs muscles (7 replicates)	61.2	3.27	56.3	830	69.8	5.47	30.9	853	42.3	5.10	74.7	852
	61.8	3.17	54.1	830	69.7	5.37	31.0	863	42.4	4.75	75.0	855
	61.2	3.45	52.2	807	69.7	5.29	30.7	865	42.9	4.99	71.5	857
	60.7	3.65	52.2	838	69.6	4.96	29.7	865	43.4	4.99	72.4	885
	66.3	3.65	51.9	841	69.7	5.42	29.9	868	43.5	4.75	70.8	889
	65.0	3.26	52.4	841	69.1	5.00	29.5	865	42.0	5.13	72.8	849
	64.9	3.89	50.9	839	69.7	4.90	29.3	859	45.4	5.42	73.2	849
Hepatopancreas (7 replicates)	157	13.9	117	750	234	11.0	94.9	653	88.4	16.5	128	554
	163	12.2	124	775	234	10.9	93.8	657	89.1	16.2	126	559
	165	11.9	123	771	239	11.0	94.4	664	93.0	16.4	129	566
	165	12.6	132	777	235	10.6	91.8	649	91.2	15.5	124	551
	163	11.6	130	778	232	11.6	90.8	658	90.5	15.4	124	550
	163	12.2	125	776	239	10.8	93.5	656	96.1	16.8	120	555
	153	12.5	124	775	247	10.6	89.4	652	84.5	14.7	119	531

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