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damienvanherp
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16.04.2014 Views

Chromium in food and drinking water 3.2. Methods of analysis 3.2.1. Food sample preparation The analyst must ensure that samples do not become contaminated during sample preparation. Wherever possible, apparatus and equipment that comes into contact with the sample should not contain chromium and should be made of inert materials, e.g. titanium or ceramic knives, agate mortar or ball mill for size reduction and homogenisation instead of stainless steel or iron equipment. These should be acid cleaned to minimise the risk of contamination (EN 13804:2013). Food samples are commonly treated in the same way as is done before consumption (washed, peeled, removal of nonedible parts). Examples of sample preparation procedures for some foodstuffs are given in EN 13804:2013. 3.2.2. Instrumental techniques 3.2.2.1. Total chromium analysis The methods of analysis of total chromium in water and food samples have been reviewed by Gomez and Callao (2006). Spectroscopy techniques flame or graphite furnace atomic absorption spectrometry (FAAS, GFAAS), inductively coupled plasma atomic emission or mass spectrometry (ICP-AES or ICP-MS) are the main techniques used followed by spectrophotometric techniques (ultra-violet (UV)- visible absorption, fluorimetry or chemiluminescence). The limit of detection (LOD) ranged from 0.5 ng/L to 8.6 µg/L in water samples depending on the preconcentration technique used (Gomez and Callao, 2006), and from 0.5 µg/L to < 250 µg/L if no pre-concentration technique is used (Table 3). EFSA Journal 2014;12(3):3595 26

Chromium in food and drinking water Table 3: LOD for total chromium in waters according to the analytical method used Detection technique Preconcentration technique (Y/N) LOD (µg/L) Reference Chemiluminescence Y 0.0005 Paleologos et al. (2003) UV-Visible N 17 Monteiro et al. (2002) FAAS N 85 Monteiro et al. (2002) FAAS N (a) < 250 EN 1233: 1996 or ISO 9174:1998 FAAS Y 8.6 Narin et al. (2008) FAAS Y 2.6 Saracoglu et al. (2002) GFAAS N (a) < 2.5 EN 1233: 1996 or ISO 9174:1998 GFAAS Y 0.020 Zhang et al. (1999) GFAAS N 0.67 Monteiro et al. (2001) GFAAS N 1.1 Monteiro et al. (2002) GFAAS Y 0.2 Pereira et al. (2004) GFAAS N 0.5 EN ISO 15586: 2004 GFAAS Y 0.3 Minami et al. (2005) GFAAS Y 0.1 Water Research Foundation (2012) ICP-OES Y 1.3 Li et al. (2003) ICP-OES N 0.5-2.5 EN ISO 11885: 2009 ICP-OES N 0.2-7 Water Research Foundation (2012) ICP-MS N 0.5 EN ISO 17294-2: 2003 ICP-MS N 0.08 Water Research Foundation (2012) GC/ICP-MS Y 0.020 Yang et al. (2004) LOD: limit of detection; UV: ultraviolet; FAAS: Flame atomic absorption spectrometry; GFAAS: Graphite furnace atomic absorption spectrometry; ICP-OES: Inductively coupled plasma optical emission spectrometry; ICP-MS: Inductively coupled plasma mass spectrometry; GC: Gas chromatography. (a): no LOD indicated, estimation based on optimal working range given. In foods, the LOD ranged from 0.23 µg/kg by ICP-MS to 90 µg/kg by FAAS (Table 4). Table 4: LOD for total chromium in foods according to the analytical method used Detection Preconcentration LOD technique technique (Y/N) (µg/kg) Reference FAAS Y 90 Yebra-Biurrun and Cancela-Pérez (2007) GFAAS N (a) < 8 EN 14082:2003 GFAAS N 20 - 80 EN 14083:2003 GFAAS N b 28 Cubbada et al. (2003) GFAAS N 20 Hammer et al. (2005) GFAAS N 1 Reczajska et al. (2005) GFAAS N 5 Figueiredo et al. (2007) ICP-AES N (a) < 0.5 Pehlivan et al. (2008) ICP-MS N (b) 13 Cubbada et al. (2003) ICP-MS N 3 Hammer et al. (2005) ICP-MS N 12 Dufailly et al. (2006) ICP-MS N 0.23 D’Ilio et al. (2008) ICP-MS N 12 Kadar et al. (2011) LOD: limit of detection; FAAS: Flame atomic absorption spectrometry; GFAAS: Graphite furnace atomic absorption spectrometry; ICP-AES: Inductively coupled plasma atomic emission spectrometry; ICP-MS: Inductively coupled plasma mass spectrometry. (a): no LOD indicated, estimation based on quantified values given; (b): given in µg/L and calculated with a sample weight of 0.3 g and a final volume of 50 mL. After pressure digestion of the food samples, inductively coupled plasma - mass spectrometry (ICP- MS) with a collision/reaction cell technology (CCT) to reduce ArC interferences, is increasingly being used, due to its multielement capacity and its sensitivity (Hammer et al., 2005; Dufailly et al., 2006; D’Ilio et al., 2008; Kadar et al., 2011). EFSA Journal 2014;12(3):3595 27

Chromium in <strong>food</strong> and <strong>drinking</strong> <strong>water</strong><br />

3.2. Methods of analysis<br />

3.2.1. Food sample preparation<br />

The analyst must ensure that samples do not become contaminated during sample preparation.<br />

Wherever possible, apparatus and equipment that comes into contact with the sample should not<br />

contain <strong>chromium</strong> and should be made of inert materials, e.g. titanium or ceramic knives, agate mortar<br />

or ball mill for size reduction and homogenisation instead of stainless steel or iron equipment. These<br />

should be acid cleaned to minimise the risk of contamination (EN 13804:2013). Food samples are<br />

commonly treated in the same way as is done before consumption (washed, peeled, removal of nonedible<br />

parts). Examples of sample preparation procedures for some <strong>food</strong>stuffs are given in EN<br />

13804:2013.<br />

3.2.2. Instrumental techniques<br />

3.2.2.1. Total <strong>chromium</strong> analysis<br />

The methods of analysis of total <strong>chromium</strong> in <strong>water</strong> and <strong>food</strong> samples have been reviewed by Gomez<br />

and Callao (2006). Spectroscopy techniques flame or graphite furnace atomic absorption spectrometry<br />

(FAAS, GFAAS), inductively coupled plasma atomic emission or mass spectrometry (ICP-AES or<br />

ICP-MS) are the main techniques used followed by spectrophotometric techniques (ultra-violet (UV)-<br />

visible absorption, fluorimetry or chemiluminescence).<br />

The limit of detection (LOD) ranged from 0.5 ng/L to 8.6 µg/L in <strong>water</strong> samples depending on the<br />

preconcentration technique used (Gomez and Callao, 2006), and from 0.5 µg/L to < 250 µg/L if no<br />

pre-concentration technique is used (Table 3).<br />

EFSA Journal 2014;12(3):3595 26

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