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Determining the total sulfite in food and beverages: faster and easier than ever

Determining the total sulfite in food and beverages: faster and easier than ever

The chances are good that if you’re reading this, you are an analytical chemist or somehow connected to the food science sector. Maybe you have had the lucky experience of measuring sulfite (SO32-) before in the laboratory. I certainly have, and the adventure regarding tedious sample preparation and proper measurement of such a finicky analyte still haunts me today, years later.

Why sulfite?

Sulfite is a preservative added to a vast range of foods and beverages to prevent browning or oxidation. Some individuals are sensitive to sulfite additives and may experience a range of allergic reactions. Therefore, both the U.S. Food and Drug Administration (FDA) and European Union (EU) laws require that the presence of sulfites be declared on food labels when the concentration exceeds 10 mg/L.

To put this into perspective, an Olympic size swimming pool can hold about 2,500,000 liters, meaning anything beyond 25 kilograms (the average mass of one young child!) would need to be reported.

So, which foods contain sulfite?

Many foods and beverages contain sulfite – whether added to prolong the freshness, or occurring naturally as a byproduct from processes like fermentation. Typically, the first things that come to mind are wine, beer, or dried fruit snacks. However, many pickled and otherwise preserved items such as sauerkraut, canned fruits and vegetables, and even frozen foods contain significant levels of sulfites. Processed meats, several condiments, and some prepared doughs are also high on the list of offenders, so beware at your next picnic!

If you think you may be sensitive to sulfites, don’t forget to check the nutrition facts, and try to avoid such foodstuffs.

How is sulfite usually measured?

Several analytical methods exist to measure sulfite in food and beverages, however they suffer from repeatability issues, and can be quite cumbersome to perform.

Traditionally, the optimized Monier-Williams (OMW) AOAC Official Method 990.28 was used for quantification of sulfite in most foodstuffs, but the method detection limit now lies at the regulatory labeling threshold. Automated discrete analysis methods have been reported for sulfite analysis, but they are limited by their strong dependence on sample matrix type. Therefore these methods are less than ideal for laboratories where sulfite analysis is required for a wide variety of food and beverage products.

Methods based on ion chromatography (IC) with conductivity detection exhibit a lack of selectivity combined with an extended analysis time due to separation challenges. A newer method developed by AOAC (Method 990.31) focuses on the use of ion-exclusion chromatography followed by electrochemical (amperometric) detection of samples.

Another issue arises concerning the sensitivity of the detector. After a few injections, fouling from contaminants rapidly decreases the electrode sensitivity. Frequent reconditioning of the working electrode is necessary due to a rising background and baseline noise, and can be accomplished in a couple of ways. Manual polishing and utilizing pulsed amperometric detection (PAD) pulse sequences are the most common choices to recondition the surface of the working electrode, while other methods opt for disposable electrodes to avoid this step altogether.

What has improved?

Metrohm has filed a patent for an innovative, fast, and accurate ion chromatographic (IC) method based on direct current (DC) mode electrochemical detection. It works with the implementation of a unique working electrode conditioning function (patent pending) in the newest version of chromatographic software (MagIC Net 3.3) offered by Metrohm. A great diversity of food and beverage products were analyzed with sulfite recovery values near 100% in all cases. Using a single, robust chromatographic method, any sample can be treated identically, saving time and making laboratory work much easier.

Sample of garlic analyzed for sulfite content (spiked: red, unspiked: black). Recovery was calculated at 100%.
(Click to enlarge)

No matter what type of sample (solid, liquid), the preparation steps are nearly identical, and much simpler to perform than ever before. Additionally, the retention time of sulfite in the method does not shift. This saves even more time for analysts as they do not have to reprocess data. Since the electrode is automatically reconditioned after each analysis, results are both reliable and reproducible. Waste from disposable electrodes is reduced, as well as costs incurred by the materials and excess working hours which would generally be spent performing other manual steps. This is truly a win-win situation for food analysis!

Benefits to QC laboratories and beyond

In real terms, this improved method allows for up to 10x the throughput of samples compared to conventional methods. Previously, the contract laboratories involved in this study could measure 5 samples, with 2 analysts per 8-hour shift (15 samples per 24 hours, if you like). With our patent-pending technique, at 10 minutes per sample, including fully automatic regeneration of the electrode surface, this allows for up to 144 samples to be analyzed every day.

Whether you work in the food and beverage industry, wastewater analysis, or in daily analytical laboratory work, you can appreciate the numerous benefits this method offers. Robustness, reproducibility, time savings, cost savings, and a simpler procedure for sample preparation across the board – are you interested? With our expertise in ion chromatography as well as electrochemistry, among other techniques, Metrohm is able to offer such cutting edge methods for the most challenging applications.

Want to learn more?

Download our free Application Note:

Sulfite determination in food and beverages applying amperometric detection

Post written by Dr. Alyson Lanciki, Scientific Editor at Metrohm International Headquarters, Herisau, Switzerland.

Special thanks are given to Miguel Espinosa, Product Manager Ion Chromatography, at Metrohm Hispania (Madrid, Spain) for his assistance in providing the laboratory data for the study.

When do I have to exchange the filtration membrane with Inline Ultrafiltration?

When do I have to exchange the filtration membrane with Inline Ultrafiltration?

Inline sample preparation is a powerful tool to make your ion chromatography analysis more efficient. Inline Ultrafiltration is an easy add-on that works for many samples. Use it for any type of sample which contains particles, like surface water, groundwater, or wastewater.

Inline Ultrafiltration by Metrohm

Ion chromatography is equipped with Inline Ultrafiltration in many branches to save time and money, e.g.:

  • Water
  • Environmental
  • Pharmaceutical
  • Food/beverage
  • Chemical
This combination increases filtration effectiveness and sample throughput. Consumables such as syringe filters are not necessary, and the workload for sample preparation in the laboratory is significantly reduced.

How often is optimal?

Customers often ask me about how often the membrane in an Ultrafiltration cell needs to be exchanged. There is no strict limit to the number of injections per membrane filter. This number strongly depends on the level of contamination of the samples.

The optimal point in time can be easily determined using our intelligent software. MagIC Net allows you to automatically integrate a check standard measurement after a certain number of samples. When the membrane filter begins to clog, the check standard data will deviate from its accepted value. MagIC Net automatically evaluates this value, and a warning message will inform you that it is time to check the system and to exchange the membrane.

Add this feature to any MagIC Net method. Define the monitoring period for the desired result.

In any case that the limit value is exceeded, a warning message will pop-up in the software. The data file is highlighted in red in the database, and the respective result is also displayed in red.

Ultimate flexibility for your needs

Monitoring the check standard is useful for several analytical methods. In this example, I explained how to use it to automatically control the performance of the Inline Ultrafiltration. Of course, the MagIC Net software has many more options for flexible methods with feedback. Contact your Metrohm representative if you want to learn more.

For more information

about inline sample preparation techniques for ion chromatography, visit our website!

Metrohm Inline Sample Preparation (MISP)

Post written by Dr. Katinka Ruth, Senior Application Specialist Ion Chromatography at Metrohm International Headquarters, Herisau, Switzerland.