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Safety evaluation of certain food additives - ipcs inchem

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SULFITES: ASSESSMENT OF DIETARY EXPOSURE 225<br />

headspace, another direct ion exchange and the third direct ion exclusion) were<br />

used to determine total sulfites in different <strong>food</strong>s. All methods produced similar<br />

results and could detect sulfites at levels as low as 1 μg/g in four <strong>of</strong> the five types<br />

<strong>of</strong> <strong>food</strong> (Lawrence et al., 1990). An HPLC method with indirect photometry was<br />

reported to be reliable to determine sulfur dioxide levels <strong>of</strong> 5–10 mg/kg in <strong>food</strong>s<br />

(Pizz<strong>of</strong>errato et al., 1990, 1998). An alternative chromatographic method based<br />

upon a combination <strong>of</strong> a modified Monier-Williams procedure and an ion<br />

chromatographic separation and quantification <strong>of</strong> total sulfite in <strong>food</strong>s was<br />

developed by Ruiz et al. (1994).<br />

A differential pulse polarographic method (AOAC International, 1995b) has<br />

been collaboratively tested and is applicable to the determination <strong>of</strong> sulfur dioxide<br />

levels <strong>of</strong> 10 mg/kg in shrimp, orange juice, peas, dried apricots and dehydrated<br />

potatoes. Alternative chemical methods for the determination <strong>of</strong> sulfites include flow<br />

injection analytical systems coupled with spectrophotometric, electrochemical and<br />

chemiluminescence detections (Sullivan et al., 1986; Lin & Hobo, 1996; Decnop-<br />

Weever & Kraak, 1997; Safavi & Haghighi, 1997; Corbo & Bertotti, 2002; Araújo et<br />

al., 2005) and capillary electrophoresis (Trenerry, 1996; Masár et al., 2004).<br />

Methods based on capillary electrophoresis have <strong>of</strong>ten been considered faster and<br />

more cost effective than other instrumental techniques, with the added advantage<br />

that most determinations can be carried out using the same fused silica capillary<br />

column. The method described by Trenerry (1996) had a limit <strong>of</strong> detection <strong>of</strong> 5 mg/<br />

kg and was found to be suitable for measuring sulfite content in a variety <strong>of</strong> <strong>food</strong>s<br />

and beverages, including samples that are not traditionally analysed by the Monier-<br />

Williams procedure. Perfetti & Diachenko (2003) described a method for<br />

determining sulfite in dried garlic. Garlic is extracted with a hydrochloric acid<br />

solution to inhibit the formation <strong>of</strong> allicin, which interferes with the determination <strong>of</strong><br />

sulfite. After cleanup <strong>of</strong> the extract on a C18 solid-phase extraction column, sulfite<br />

is converted to hydroxymethylsulfonate by adding formaldehyde and heating to<br />

50 °C. Hydroxymethylsulfonate is determined by reversed-phase ion-pairing liquid<br />

chromatography with post-column detection. Recovery <strong>of</strong> hydroxymethylsulfonate<br />

from spiked garlic averaged 94.8%, with a coefficient <strong>of</strong> variation <strong>of</strong> 3.8%.<br />

In conclusion, several methods are available for the determination <strong>of</strong><br />

sulfites in <strong>food</strong>s and beverages, the choice <strong>of</strong> method depending, among other<br />

factors, on the matrix to be analysed and the expected concentration <strong>of</strong> sulfite.<br />

The most common methods in use to date involve distillation <strong>of</strong> sulfur dioxide from<br />

a highly acidified sample, followed by titration, colorimetric, polarographic or ion<br />

chromatographic determination. The iodometric titration methods are not<br />

considered very useful for low analyte concentrations, and the enzymatic methods<br />

using commercial kits <strong>of</strong>fer less sensitivity. To fill the gap when the Monier-Williams<br />

method is not applicable, alternative methods based on HPLC, ion chromatography,<br />

capillary electrophoresis and flow injection analytical techniques have been<br />

developed. In this context, various detection techniques, such as spectrophotometry,<br />

amperometry, potentiometry and chemiluminescence, have been<br />

applied. Whatever test procedures have been adopted by laboratories, they need<br />

in-house validation, and the results should be compared with a reference method.<br />

It is essential for laboratories to implement a well documented internal quality control

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