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Comparative efficacy of two standard methods for determination of iron and

zinc in fruits, pulses and cereals

Article in Journal of Food Science and Technology -Mysore- · July 2013

DOI: 10.1007/s13197-013-1088-6

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J Food Sci Technol (February 2015) 52(2):1096–1102
DOI 10.1007/s13197-013-1088-6

ORIGINAL ARTICLE

Comparative efficacy of two standard methods

for determination of iron and zinc in fruits,
pulses and cereals
H. M. Jajda & K. G. Patel & S. R. Patel & V. H. Solanki &
K. N. Patel & Susheel Singh

Revised: 27 June 2013 / Accepted: 1 July 2013 / Published online: 7 July 2013
# Association of Food Scientists & Technologists (India) 2013

Abstract Micronutrients are essential elements needed in micronutrient Fe and Zn are an essential mineral, vital to
small amounts for adequate human nutrition and include human metabolism, growth and immune function (Aggett
the elements iron and zinc. Both of these minerals are essen- and Comerford 1995). Iron (Fe) and zinc (Zn) are involved
tial to human well-being and an adequate supply of iron and in the function of several enzymes and are essential for
zinc help to prevent iron deficiency anaemia and zinc defi- maintaining health throughout life (Uauy et al. 1998). Iron
ciency, two prevalent health concerns of the developing deficiency is the most prevalent single nutritional deficiency
world. The levels of zinc and, iron were measured in the in the world and is the main cause of anemia in infants,
Banana, Papaya, Rice, Finger millet, Soybean and Urdbean. children, adolescents, and women of childbearing age
Standard Atomic absorption spectroscopy (AAS) method (DeMaeyer and Adiels-Tegman 1985). Zinc deficiency may
was also applied to all the samples for zinc and iron analysis be widespread in developing countries, but it is under-
and compared with inductively coupled plasma mass spec- recognized due to lack of sensitive biomarkers of Zn status.
troscopy (ICP-MS). It was observed that there was no matrix In addition, there is scarce information on Fe and Zn intakes in
interference affecting the determination of both elements our population. Accurate estimation of both the nutrient is
interested in all the samples analyzed. Average concentration very much essential and its value in same food material is
relative standard deviation and standard deviation were used varying with method adopted. For the elemental analysis there
for the statistical evaluation of the results for both elements. are a number techniques we could use, including spectromet-
Correlation coefficient was used as statistical model to compare ric, flame and furnace AA (Atomic Absorption) and ICP-MS
both the techniques. (ICP Mass Spectrometry). Selection of appropriate method to
quantify the nutrient is an important task. Inductively coupled
Keywords ICP-MS, AAS . Zinc . Iron . Banana . Papaya . plasma-mass spectrometry (ICP-MS) is a multi-element anal-
Rice . Finger millet . Soybean and Urdbean ysis technique, which provides high selectivity and lower
detection limits than other techniques, such as inductively
coupled plasma optical emission spectrometry (ICP-OES),
Introduction AAS and spectrometry (Tyler et al. 2002). These characteris-
tics make ICP-MS an excellent tool for detailed characterisa-
Nutritional quality is an important characteristic of food crop tion of the elemental composition of numerous samples.
varieties that determines their functional value in the human When the highest quality of results is needed, the isotope
diet. Micronutrient concentration in turn is an important dilution mode of analysis is the choice, whereas the quantita-
component of nutritional quality especially for staple crops tive mode of analysis is the default strategy (Laborda et al.
in developing countries (Frossard et al. 2000). Among 2001). The quantitative mode of analysis in ICP-MS requires
external calibration with standards of each element to be
determined. This strategy is time consuming and it is not easy
H. M. Jajda (*) : K. G. Patel : S. R. Patel : V. H. Solanki : to have a complete set of the multi-element standards required
K. N. Patel : S. Singh
for the calibration. A third option, the semi-quantitative mode
Food Quality Testing Laboratory, Navsari Agricultural University,
Navsari 396450, India of analysis, is a versatile application of ICP-MS that it is
e-mail: [email protected] claimed to allow the determination of about 80 elements with
J Food Sci Technol (February 2015) 52(2):1096–1102 1097

errors <20 % for most elements (Laborda et al. 2001; quality testing laboratory, Navsari agricultural university,
Soldevilla et al. 1998; Amarasiriwardena et al. 1997). This Navsari-396450 (Gujarat), India.
methodology has been successively applied to samples of
different nature and origin, like biological (Amarasiriwardena
et al. 1997; Krushevska et al. 1996; Alonso et al. 1997), Result
environmental (Alonso et al. 1997), industrial (Hu et al.
1997), food (Castillo et al. 1999; Jakubowski et al. 1999; Iron and zinc content of rice
Castineira et al. 2001) and plastics (Fordham et al. 1995)
samples. The semi-quantitative analysis software available Iron content was found to be 66.55 ppm to 71.37 ppm in rice
for commercial ICP-MS instrumentation (e.g. TotalQuant II samples analyzed by ICP-MS and 66.45 ppm to 72.24 ppm
from Perkin-Elmer) has facilitated the rapid acquisition of (range) by AAS. The average iron content in all rice samples
analytical data by correcting automatically isobaric and molec- was found to be nearly similar 69.20 ppm by ICP-MS and
ular interferences as well as relative isotope abundances. This 69.55 ppm by AAS. Zinc content was found to be 30.95 ppm
type of analysis is based on a pre-calibrated internal response to 49.1 ppm in rice samples analyzed by ICP-MS and
(defined as ions per second per concentration unit) for all 31.52 ppm to 48.8 ppm by AAS. The average zinc content
elements, which can be update with a single-point calibration in all rice samples was found to be 37.02 ppm by ICP-MS
(Amarasiriwardena et al. 1997) and 38.32 by AAS (Table 1).
In present study we have compared inductively coupled
plasma mass spectrometry (ICP-MS), a latest technique can Iron and zinc content of finger millet
detect the elements at ppt level with atomic absorption spec-
trometry (AAS) for Fe and Zn determination in six different The iron and zinc content of finger millets is presented in
food material like Banana, Papaya, Rice, Finger millet, Table 2. The results showed that all samples contained detect-
Soybean and Urdbean. able amounts of iron and zinc. Iron content varied between
samples from 60.0 ppm to 95.9 by ICP-MS and 59.4 ppm to
99.3 ppm by AAS. The average iron content in all the finger
Material and method millets samples was found to be nearly similar 73.22 ppm by
ICP-MS and 73.72 ppm by AAS. Zinc content was found to
Sampling be 16.1 ppm to 23.1 ppm in finger millets samples analyzed
by ICP-MS and 16.7 ppm to 23.9 ppm by AAS. The average
About 18 samples of banana and 36 samples of papaya fruits zinc content in all the finger millets samples was found to be
were collected from Navsari agricultural university farm and 18.69 ppm by ICP-MS and 19.3 by AAS.
well managed farm of south Gujarat, India. Samples were
physically cleaned by rinsing with deionised water to remove Iron and zinc content of papaya
dirt and other extraneous filth. Fresh pulp of banana and
papaya were used for analysis. Whereas 15 samples of rice, Iron content was found to be 43.6 ppm to 70.5 ppm in papaya
60 samples of finger millet, 27 samples of black gram and 27 samples analyzed by ICP-MS and 37.5 ppm to 71.8 ppm by
samples of soybean were collected from Navsari agricultural AAS. The average iron content in all papaya samples was
university farm and well managed farm of south Gujarat, found to be 51.04 ppm by ICP-MS and 52.04 ppm by AAS.
India. Seed samples were dried and powdered to analyzed Zinc content was found to be 6.9 ppm to 12.4 ppm in papaya
zinc and iron content. samples analyzed by ICP-MS and 7.8 ppm to12.6 ppm by
AAS. The average zinc content in all papaya samples was
Sample analysis found to be 9.45 ppm by ICP-MS and 10.07 by AAS
(Table 3).
About 0.5 g of sample was weighed using a Teflon vessel,
and then a mixture of concentrated HNO3 and HCLO4 (10:4) Iron and zinc content of banana
was added. The digestion vessel was closed and heated in the
microwave oven. The obtained solutions were allowed to cool The iron and zinc content of banana is presented in Table 4.
at room temperature, and then were filtered by Whatman No. The results showed that all samples contained detectable
1 (110 mm pores size) filter paper into a 25 mL in volumetric amounts of iron and zinc. Iron content was found to be from
flask and make the volume using double distilled deionized 16.8 ppm to 26.7 ppm by ICP-MS and 17.5 ppm to 27.9 ppm
water. These extract were used for determination of Fe and Zn by AAS in all the banana samples analyzed. The average iron
through AAS (Electronics Corporation of India Ltd. AAS content in all the banana samples was found to be nearly
4141) and ICP-MS (Perkin Elmer series Elan-900) at food similar 22.43 ppm by ICP-MS and 23.05 ppm by AAS. Zinc
1098 J Food Sci Technol (February 2015) 52(2):1096–1102

Table 1 Analysis of iron and

zinc in rice by ICP-MS and AAS Name of sample Iron Zinc

Concentration Concentration Concentration Concentration

(ICP-MS) ppm (AAS) ppm (ICP-MS) ppm (AAS) ppm

Rice 1 68.84 68.12 49.1 48.8

Rice 2 71.37 72.24 37.4 38.5
Rice 3 71.37 72.19 36.1 36.7
Rice 4 67.89 68.75 30.95 31.52
Rice 5 66.55 66.45 31.56 32.12
Avg. Conc. Std. deviation 0.1 2.5 0.01 1.2
Avg. Conc. Relative std. deviation 1.0 5.9 0.9 3.8
Range 66.55–71.37 66.45–72.24 30.95–49.1 31.52–48.8
Mean 69.20 69.55 37.02 38.32
Correlation 0.969589 0.965291

content was found to be 8.7 ppm to 12.1 ppm in banana AAS. The average zinc content in all the banana samples was
samples analyzed by ICP-MS and 9.4 ppm to 12.9 ppm by found to be 10.58 ppm by ICP-MS and 11.6 by AAS.

Table 2 Analysis of iron and

zinc in finger millet by Name of sample Iron Zinc
ICP-MS and AAS
Concentration Concentration Concentration Concentration
(ICP-MS) ppm (AAS) ppm (ICP-MS) ppm (AAS) ppm

Finger millet 1 95.9 99.0 23.1 23.9

Finger millet 2 93.2 95.3 20.7 21.3
Finger millet 3 64.5 66.6 20.5 21.2
Finger millet 4 60.8 62.6 19.6 20.1
Finger millet 5 87.3 90.6 19.3 19.9
Finger millet 6 97.1 97.8 19.3 19.8
Finger millet 7 80.9 81.0 19.6 20.2
Finger millet 8 66.7 67.3 19.1 18.9
Finger millet 9 72.6 72.1 17.3 17.8
Finger millet 10 60.0 59.4 18.6 19
Finger millet 11 69.3 70.5 19.9 20.2
Finger millet 12 65.7 66.9 17.6 18.3
Finger millet 13 71.4 72.5 18.3 18.9
Finger millet 14 63.8 64.6 18.6 19.4
Finger millet 15 60.9 62.4 17.3 17.9
Finger millet 16 76.5 64.4 17.6 18.9
Finger millet 17 64.4 66.2 17.3 18
Finger millet 18 69.8 70.6 16.1 16.7
Finger millet 19 80.6 82.4 16.2 17.1
Finger millet 20 63.0 62.3 17.8 18.5
Avg. Conc. SD. 0.1 3.3 0.1 8.6
Avg. Conc. RSD. 1.2 6.3 0.8 4.1
Range 60.0–95.9 59.4–99.3 16.1–23.1 16.7–23.9
Mean 73.22 73.72 18.69 19.3
Correlation 0.9688 0.985723
J Food Sci Technol (February 2015) 52(2):1096–1102 1099

Table 3 Analysis of iron and

zinc in Papaya by ICP-MS Name of sample Fe (ppm) Zn (ppm)
and AAS (Papaya)
Concentration Concentration Concentration Concentration
(ICP-MS) ppm (AAS) ppm (ICP-MS) ppm (AAS) ppm

Papaya 1 47.0 48.2 9.2 9.9

Papaya 2 36.9 37.5 10.1 11.2
Papaya 3 43.6 45.3 12.4 12.9
Papaya 4 43.6 44.9 12.4 13.1
Papaya 5 53.7 54.8 11.5 12.6
Papaya 6 50.3 51.5 9.6 10.2
Papaya 7 51.2 51.9 7.1 7.9
Papaya 8 50.3 52.3 6.9 7.8
Papaya 9 70.5 71.8 8.3 8.9
Papaya 10 53.3 54.6 8.7 9.8
Papaya 11 50.3 51.4 9.3 10.1
Papaya 12 63.8 65.3 7.9 8.5
Avg. Conc. Std. deviation 0.7 10.2 0.5 3.4
Avg. Relative std. deviation 0.1 13 0.1 0.7
Range 43.6–70.5 37.5–71.8 6.9–12.4 7.8–12.6
Mean 51.04167 52.04167 9.45 10.075
Correlation 0.975332 0.94034

Iron and zinc content of soybean Iron and zinc content of urdbean

The soybean samples contain 71.8 ppm to 200.4 ppm iron The iron and zinc content of urdbean is presented in Table 6.
and 40.9 ppm to 60.3 ppm zinc when analyzed by ICP-MS The results showed that all samples contained detectable
where as by AAS analysis it was found to be 78.6 ppm to amounts of iron and zinc. Iron content was found to be
210.6 ppm iron, 39.8 ppm to 61.9 ppm zinc respectively. The from 88.8 ppm to 221.9 ppm by ICP-MS and 86.1 ppm to
average iron content found by ICP-MS was 123.73 ppm 212.5 ppm by AAS in all the urdbean samples analyzed. The
almost similar with, it was found to be 123.23 ppm by average iron content in all the urdbean samples was found to be
AAS in all the soybean samples. The average zinc content nearly similar 142.2 ppm by ICP-MS and 143.5 ppm by AAS.
was found to be 50.7 ppm by ICP-MS and 51.1 ppm by AAS Zinc content was found to be 32.9 ppm to 50.0 ppm in urdbean
in all soybean samples (Table 5). samples analyzed by ICP-MS and 34.1 ppm to 54.9 ppm by

Table 4 Analysis of iron and

zinc in Banana by ICP-MS Name of sample (Banana) Fe (ppm) Zn (ppm)
and AAS
Concentration Concentration Concentration Concentration
(ICP-MS) ppm (AAS) ppm (ICP-MS) ppm (AAS) ppm

Banana 1 26.7 27.2 12.1 12.8

Banana 2 18.1 18.9 8.7 9.4
Banana 3 23.5 24.2 12.0 12.9
Banana 4 16.8 17.5 10.1 10.8
Banana 5 26.8 27.6 10.1 11.1
Banana 6 26.7 27.9 11.5 12.6
Avg. Conc. Std. deviation 0.5 8.5 0.6 4.2
Avg. Relative std. deviation 0.1 12 0.2 0.8
Range 16.8–26.7 17.5–27.9 8.7–12.1 9.4–12.9
Mean 22.43333 23.05 10.58333 11.6
Correlation 0.967581 0.968975
1100 J Food Sci Technol (February 2015) 52(2):1096–1102

Table 5 Analysis of iron and

zinc in Soybean by ICP-MS Name of sample Fe (ppm) Zn (ppm)
and AAS (Soybean)
Concentration Concentration Concentration Concentration
(ICP-MS) ppm (AAS) ppm (ICP-MS) ppm (AAS) ppm

Soybean 1 199.7 210.6 56.3 58.6

Soybean 2 114.0 125.8 50.7 50.0
Soybean 3 200.4 186.5 60.2 61.3
Soybean 4 111.3 102.6 48.7 50.8
Soybean 5 88.9 80.1 52.4 48.9
Soybean 6 99.5 97.3 40.9 39.5
Soybean 7 81.7 85.4 46.5 49.7
Soybean 8 71.8 78.6 40.9 39.8
Soybean 9 146.3 142.2 60.3 61.9
Avg. Conc. Std. deviation 0.9 3.5 1.2 4.3
Avg. Relative std. deviation 0.1 1.3 0.1 2.3
Range 71.8–200.4 78.6–210.6 40.9–60.3 39.8–61.9
Mean 123.7333 123.2333 50.7 51.1
Correlation 0.981578 0.96789

AAS. The average zinc content in all urdbean samples was of rice genotypes for iron and zinc concentration. They found
found to be 43.1 ppm by ICP-MS and 43.7 by AAS. Iron concentration ranged from 6.2 ppm to 71.6 ppm and
zinc from 26.2 ppm to 67.3 ppm in their study which is
similar to our study. Similarly Shashi et al. (2007) found
Discussion 36.00 ppm to 73.00 ppm iron content and 18.00 ppm to
23.00 ppm zinc in finger millet genotype analyzed. In case
Iron and zinc contents of all samples of Iron and zinc content of banana, Mohpatara et al. (2010)
were found 8.3 ppm iron and 2.3 ppm zinc in banana. Rani
Iron and zinc content reported in this study reveals that iron et al. (2008) reported 84.00 ppm to 112.00 ppm iron and
and zinc content falls in the ranges reported in the previous 71.00 ppm to 79.00 ppm zinc in analyzed soybean genotype,
studies. Anuradha et al. (2012) have analyzed 126 accessions supporting our result.

Table 6 Analysis of iron and

zinc in Urdbean by ICP-MS Name of sample Fe (ppm) Zn (ppm)
and AAS (Urdbean)
Concentration Concentration Concentration Concentration
(ICP-MS) ppm (AAS) ppm (ICP-MS) ppm (AAS) ppm

Urdbean 1 204.2 212.5 36.4 38.5

Urdbean 2 90.3 95.3 38.9 37.4
Urdbean 3 96.2 95.8 48.6 47.6
Urdbean 4 208.9 211.6 42.9 45.8
Urdbean 5 144.4 159.2 48.4 48.2
Urdbean 6 132.1 139.7 48.1 46.2
Urdbean 7 93.5 90.9 42.0 40.6
Urdbean 8 221.9 200.6 50.0 54.9
Urdbean 9 88.8 86.1 32.9 34.1
Avg. Conc. Std. deviation 0.7 2.1 0.4 6.2
Avg. Relative std. deviation 0.1 5.3 0.1 1.9
Range 88.8–221.9 86.1–212.5 32.9–50.0 34.1–54.9
Mean 142.2 143.5 43.1 43.7
Correlation 0.983113 0.932699
J Food Sci Technol (February 2015) 52(2):1096–1102 1101

Comparison of ICP and AAS methods last section, we discussed both methods to determine iron
and zinc, which clarifies that improving determination tech-
The two methods used for mineral analysis were reliable and nique, should take into account many things like sensi-
gave similar results as shown by low coefficients of variation tivity, efficiency, cost, etc. By comparing ICP-MS and
and highly significant correlations between methods. In terms AAS, we determined that ICP-MS was better but more
of repeatability of the iron analysis in six different matrices expensive, which helped determine that the most impor-
shown average concentration standard deviation and relative tant thing to do in any analysis is to compare the
standard deviation 0.5 and 0.55 respectively for ICP-MS while different methods and then choose the best one of them
5.01 and 7.3 respectively for AAS method which revealed that that works.
ICP-MS is more precise technique than AAS. Similarly in zinc
analysis average concentration standard deviation and relative
standard deviation found to be 0.56 and 0.36 respectively for
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