Food Labels, Naturally

By Michael Pickering

While making my selections at the grocery store, I am often struck by the myriad of claims presented on food packaging.  I wonder what exactly qualifies a peach jam as “organic,” or a powdered diet beverage as “natural?”  made with natural ingredientsOr when is a manufacturer allowed to claim specific health benefits from their product, or to declare that their food is a “good source” of a nutrient? My own experiences and growing curiosity have led me down this rabbit hole of exploration, and in sharing my discoveries I hope to add transparency to your next grocery trip.

At one time, specific nutrient descriptors were only loosely defined and the serving size was up to the discretion of the producer.  As you’d expect, this led to wildly different nutrition labels from one manufacturer to the next, even when comparing the same product.  Although there are still several misleading areas of food labeling (to be discussed), the regulatory push to standardize nutrient labeling, create serving sizes that reflect typical consumption, and plainly list common allergens has benefited today’s consumers.  It allows us to quickly compare two brands of the same product and determine the nutritional value of each.

Consistent serving sizes by product are now defined and enforced, and the serving measurements are required to be printed in both metric and common household units.  handheld labelHealth claims are required to follow more exacting guidelines – the amount of nutrient required to be present in order to claim a direct link to the health-related condition has been clearly defined.  For example, in order to print claims about reducing the risk of osteoporosis, a food must contain at least 200 milligrams of calcium, in a form that can be readily absorbed into the body.

In addition to specific requirements for claiming health benefits, manufacturers also must follow specific guidelines when using phrases like “free” or “fresh” or “source.”  For example: labeling a food as “Sodium Free” requires it to contain less than 5 mg of sodium per serving and not have any ingredient that is sodium chloride, and if the food occurs normally as being sodium free without additional processing or alteration, that must be disclosed.

During the last couple of years, I’ve seen a growing number of labels declaring foods to be “gluten-free.”  In line with my observations, the FDA recently implemented clear requirements for “gluten-free,” and any food that fails to meet the 20 ppm (20 mg of gluten in 1 kg of food) maximum will be prosecuted as misbranded.  Gluten-containing grains (wheat, rye, and barley) must be absent completely from the ingredient list, as well as any ingredient derived from a gluten-containing grain (such as flour).   In fact, I learned that food producers must now clearly label whether a product contains any of the most common allergens, which are responsible for 90% of all food allergic reactions.

Most Common Food Allergens
Milk Peanuts Shellfish Tree Nuts Eggs Fish Soy Wheat

Organic foods follow strict criteria and regulation by the National Organic Program (USDA).  To be labeled “organic,” a food must consist of at least 95% organically produced ingredients.  There is a list of nonagricultural substances approved for use in the remaining 5% (which are not commercially available in organic form).  Organic foods are produced using approved organic farming methods, which prohibit the use of synthetic fertilizers and pesticides.  They also may not be irradiated or genetically modified.usda organic

The discussion of “organic” foods leads us organically into a discussion of “natural” foods, and here is where food labeling begins being less transparent.  The FDA defines “natural flavoring” in great detail, including specifying that a natural flavor may only be expressed in the food’s label if that flavor simulates the food from which it is derived.  For example, using a natural flavoring derived from an apple to make a juice taste of strawberries requires the manufacturer to either label it as “artificially flavored” or else to label the juice as containing “natural apple flavor.”  While on the subject of juices, the FDA declares that if a juice drink is less than 100% juice, it is not allowed to declare itself neither “100% natural” nor “100% pure.”free of stuff tags

Interestingly, this is where the FDA guidance for “natural” comes to a halt.  There is no FDA definition or regulation of “natural” on food labels, beyond the previously discussed flavors.  The USDA has limited the use of “natural” to only indicate a product containing no artificial ingredient or added color and only minimal processing, but this only applies to the USDA-governed meat, poultry, and eggs.  The FDA has a longstanding policy (not a formal definition) to consider the term “natural” to mean that nothing synthetic or artificial (including all color additives regardless of source) has been added. Without further regulation, foods labeled “natural” can include high fructose corn syrup, genetically engineered ingredients, and any other plant-derived substances such as flavors or sweeteners.

When comparing foods as “organic” versus “natural,” I like to think of the analogy of a person describing themselves as “religious” versus “spiritual.”  Much like a religious person follows particular guidelines for their practice, so too is organic food grown with specific procedures and outcomes in mind.  In comparison, I think of a spiritual person as more fluid, with fewer specific rituals or at least less commonly-defined ones, and that would hold true for natural foods.  Natural foods are not rigidly regulated, which results in each manufacturer creating their own set of beliefs for what determines how “natural” their foods are.

Food for thought, when you are next out grocery shopping.

AOAC International Annual Meeting in Boca Raton

This year’s meeting was held at the Boca Raton Resort in Florida.  sunsetWe had a booth this year as usual, and we presented our FREESTYLE ThermELUTE system, which is a great new automated system for fast and sensitive Mycotoxin analysis. We also shared some details about this new system in our Vendor presentation and our poster titled “Integrated Analysis and Automated Sample Cleanup of Aflatoxin B/G, M1, Ochratoxin A”banyon tree

In addition to ThermELUTE, Laszlo Torma and Maria Ofitserova were on hand to participate in several community meetings and Expert Review Panels and to present a second poster.

After the exhibition ended on Tuesday afternoon, we stayed to listen to Wednesday’s talks and to present our second poster on Glufosinate, titled simply, “Glufosinate and Glyphosate in Water”  While this herbicide is not necessarily a new topic, it’s certainly a challenging one, and with the developing resistance of the unwanted plants (i.e. weeds) to Glyphosate, growers are turning to this herbicide.

As a team, we sat in on a few sessions; this editor sat in on two:

Honey Production & Veterinary Drug Contamination: Fate & Control in which some new methods for analyzing antibiotics in honey were presented. One particularly interesting presentation highlighted the challenges of finding standards for several degradation products of the antibiotics in the honey.

Analytical Challenges with Chemicals of Emerging Concern to Test Food Quality and Safety: Presentations included studies about the uptake of Emerging contaminants (i.e. flame retardants, diphenhydramine) by crops using reclaimed water, and an interesting technique using metabolomics to determine the authenticity of herbs and spices. A third presenter described their analytical challenges when facing illegal food dyes, such as Rhodamine B in imported products. This last presentation was rather frightening due to the prevalence of these dyes in products from developing countries which are finding their way into our food supply.

Outside of the meeting rooms, the resort is located in a very affluent area of Boca Raton. It was rumored that Oprah Winfrey is a member of the golf club there. Indeed, while taking a short walk around the grounds, we saw a Ferrari, a Mazerati, and a Bentley. Not to mention several Mercedes Benz and Porsche. On the water were several megayachts, mega yachtand an Oyster sailing yacht. oysterThe sailboat included a paid crew, bow thrusters and electric winches, all of which would be very much appreciated by this editor on our boat (although some would argue that such conveniences are “cheating”).

All in all, it was a good meeting. We enjoyed seeing old friends and making new ones.  We look forward to the 2015 meeting in Los Angeles, California.

boca view east

boca view north


Cleanup Columns for Aflatoxin M1

Continuing to build on our LCTech product line for Myctoxin analysis, we are very happy to report that we now have cleanup columns for M1 in milk and dairy products.Milch

Borrowing text from our partners at LCTech:

LCTech has developed the immunoaffinity columns AflaCLEAN™ Select M1 and AflaCLEAN™ SMART M1 for the clean-up for aflatoxin M1 from milk and dairy products in the format of 3 mL or the practical SMART format to simplify the sample preparation for the analysis of food.

Both formats of the columns have a loading capacity of 100 ng aflatoxin M1 and convince with excellent recoveries ≥ 90%.

The immunoaffinity column AflaCLEAN™ Select M1 can be automatically processed with the AcceCLEAN™ or the FREESTYLE™ robotic system. The SMART columns impresses especially in combination with the FREESTYLE™ ThermELUTE™ providing an automated handling from extract to the chromatogram with a sample throughput of more than 500 samples per week and a reduced solvent consumption at the same time.

Also, LCTech have on their website a great resources called Matrix of the Month. Be sure to click over and check it out.

Please don’t hesitate to contact us if you have any questions:

Chromatography Quiz #17

Chromatography Quiz #16 Results:

We would like to congratulate our grand prize winners of our last newsletter’s Blast from the Past Picture Quiz: Richard Dickerson from Eurofins Nutritional Analysis Center, della terra gourmet gift setNarjes Ghafoori from LA County Environmental Toxicology Laboratory, Tom Schneider from Suffolk County Water Authority, Dr. Pravish Tiwari from Cipla, Matthew Hartz from Eurofins Eaton Analytical, and Dr. Paul Levy from the Children’s Hospital at Montefiore!

They have each won and will shortly be receiving: a Della Terra Gourmet Gift Set!!  The 25-year-aged balsamic vinegar and signature extra virgin olive oil are presented elegantly in this delightful collection by the Della Terra family, and delivered courtesy of

We would like to thank all of you for your submissions!

The correct answer for the flashback picture:

Despite Michael’s adamant protests, the photographer insisted on prominently displaying the Trione bottles during the photo shoot for the fluorometer detector.  Seeing as how Trione is not a fluorescent reagent, this choice was almost as embarrassing as the quote “Gilson’s 121 is the best fluorometer I’ve used” boldly stated in the original advertisement.  The year this Gilson ad was published, Michael was approached (good-naturedly) by every other fluorometer manufacturer at Pittcon.

Thank you!

Pickering Labs

Chromatography Quiz #17:

Oct 1, 2014, Editor’s Note: We discovered a typo. Originally, we listed the Reactor 1 temperature at 100°C. It should be 36°C 

Identify the error made when running the Glyphosate chromatogram below and win a prize!  Simply email your answer as well as your full contact information to Rebecca at by November 1st, 2014 in order to win.  You will receive email confirmation that your submission has been received.  The troubleshooting answer and winner congratulations will be published in the next issue (to be anonymous, please notify Rebecca in submission).

Glyphosate Analysis for US EPA Method 547

Pickering Standard: 1700-0080 Glyphosate Test Mixture, 2.5 µg/mL, 10 µL injection

Pickering Column: 1954150 Cation-exchange Column for Glyphosate, 4x150mm

Normal Operating Conditions: (for reference only, condition changes may be reflected in chromatogram)

Column Temperature: 55°C

Flow rate: 0.4 mL/min

Eluant Gradient:

eluant gradient for quiz 17

Post-column conditions:

Reagent 1: Oxidizing reagent – 100 uL of 5% Sodium Hypochlorite in 950 mL of GA116

Reagent 2: 100 mg of OPA, 2 g Thiofluor™ in 950 mL of GA104

Reactor 1: 36 °C, 0.5 mL

Reactor 2: ambient. 0.1 mL

Reagent flow rates: 0.3 mL/min

Detection: Fluorometer ex 330 nm, em 465 nm

Troubleshooting Chromatogram:glyphosate troubleshooting chromatogram quiz 17

Reference Chromatogram:glyphosate reference chromatogram quiz 17

The Origins of Trione

By Mike Gottschalk

Michael Pickering got the idea for Trione on his first day as a research chemist at Durrum Instruments back in 1976. While they were showing him their Amino Acid analysis instrument they opened the refrigerator to reveal the eluents and reagents in their reservoirs. One solution was red. He asked, “What’s the red stuff?” The reply was that it was the ninhydrin reagent. He asked, “Why is it red, ninhydrin isn’t red!” The answer was no one knew. He said, show me the instrument later, take me to documents, “I want to see the formula for the ninhydrin.” Seeing the formula reveal that Stan Moore’s recipe included Dimethylsulfoxide (DMSO) as the essential water miscible organic solvent. While DMSO is a great solvent, it’s also reactive, and responsible for the secondary reactions that lead to the background red color.

Before join Durrum Instruments Michael had followed the work of George Olah in Carbonium ion chemistry. He’s the guy who developed “magic acid” which could protonate methane to make CH5+. His solvent of choice was sulfolane, a water miscible, non-reactive organic solvent.

The idea was born. However, Durrum Instruments had no interest in making consumables. The company where he next worked was Spectra Physics which also had no interest in making consumables. But on his starting interview with personal he was required to list his ideas that he thought were patentable. Number one was Trione.

Early on, he enlisted the help of Bertum Russel, a chemistry patent attorney to get the patent for Trione. Bertum’s conditions were “If you think you’re going to make money by licensing this I won’t waste your money, but if you are going to make it, I’ll get you a patent.”

That same year, Michael contacted Stan Moore at Rockefeller University to get his assessment after using Trione. Afterall, what better way to start a business than to have the endorsement of one of the researchers who developed the original ninhydrin. Stan said, “You should do well with this but I have post-docs making ninhydrin for me every day so I won’t need to buy it.”

Undeterred, Michael gave seminars and workshops thought the analytical community and soon acceptance by the analytical chemists made Trione the best in class ninhydrin for Amino Acid analysis it is today.

Pittcon 2014

This year’s Pittcon was held in Chicago, Illinois from March 3-6.

The overwhelming theme of this meeting was COLD. Winter was still very present in Chicago that week with temperatures dropping well below freezing.chicago 2014

But despite the cold, there was a good turnout and it was a successful show. As usual, we had on hand our Pinnacle PCX and our post-column applications. We also had our FREESTYLE Sample Cleanup system. This is always a great show for meeting distributors, suppliers, customers. Nowadays Pittcon is as much (if not more) about networking and meetings as it is about finding new equipment.

Beer sampler

The sampler at 18th Street Brewery

We usually try to find some adventure or other on the Sunday before the show starts, and this year was no exception. This year, we braved the cold and the snow to venture out to Gary, Indiana!  Before Pittcon, this editor had visited 45 of the 50 US States. Indiana was one of 5 remaining.

Waiting for the train under McCormick Place

Waiting for the train under McCormick Place

The requirements for the day were: 1) easy to get to without a car 2) be located outside the city limits of Chicago and 3) have a restaurant/bar close to the train station.  After some internet research, the 18th Street Brewery in Gary, IN seemed to fit the bill perfectly!

you are beautiful

We were told the Aquatorium is a fun place in summer

We took the South Shore Line from McCormick Place  out to Gary, where we trudged through a foot of snow to the 18th Street Brewery.  It turns out this is a wonderful brewery with good beer and friendly folks. And they even had a grill out back which was cooking up kielbasa sausage with kimchi. If you’re ever in Chicago and need a change of pace, or are in northern Indiana, it’s worth a stop.

All in all it was a good trip and a successful meeting. But I’m glad Pittcon 2015 will be in New Orleans…

Joint Western & Eastern Canada Workshop

Pickering Laboratories participated in the first joint Western & Eastern Canadian Trace Organic Workshop, held in Guelph, Ontario.   We shared a table with our Canadian distributor, Chromatographic Specialties. The meeting was well attended and there were many interesting talks. The purpose of the meeting is to share the latest methods and information about trace analysis — for a wide range of analytes from pesticides, to dioxins, to PCBs, flame retardants, and surfactants.

We presented two posters:

Cleanup and Determination of Aflatoxins in Peanuts and Peanut Butter using Immunoaffinity Cleanup with HPLC- Post-column UVE Photochemical Derivatization


Glyphosate analysis in soy beans, corn and sunflower seeds by HPLC with post-column derivatization and fluorescence detection

In addition to the two posters, we had the latest information on the FREESTYLE Sample Preparation system, and in particular the ThermELUTE module, for rapid and sensitive cleanup and analysis of Aflatoxins and Ochratoixn A.

In the News: Phthalates

By Michael Pickering

While reading the NY Times one morning in March, I came across an article titled “A Plastic Threat to Male Fertility” in the Science Times section. Having encountered phthalates in the past, I was curious to read further.

Federal researchers recently spent four years tracking 501 couples who were trying to have children. The goal of their study was to assess the impact of everyday chemicals on fertility. While both men and women were exposed to known toxins, men appeared much more likely to suffer fertility problems as a result.

“Anything you can think of that’s testosterone-dependent is likely to be affected.”   – Heather Patisaul, North Carolina State University

The gender disparity was most significant when it came to phthalates. This group of petrochemicals finds its way into many commercial products. Phthalates are among a group of compounds known as endocrine disruptors. As the endocrine system controls the production and distribution of hormones in the body, they have been implicated in a range of health problems. Unlike many of the study’s other industrial toxins that bio-accumulate, phthalates are metabolized within hours of ingestion. However, their pervasiveness in the environment means almost constant exposure, which increases their impact.

Among the myriad uses for phthalates are as plasticizers (rendering polymers flexible rather than brittle) and in cosmetics, where they improve smoothness of flow upon application.

Partial List:

  • Cosmetics
  • Plastics
  • Household products
  • PVC pipes
  • Hospital tubing
  • Medicine (pills, capsules)
  • Air filters, residential and commercial

While the evidence for an effect on male fertility is compelling, it is still difficult for researchers to gauge the full impact these prevalent phthalates are having. If you want to minimize your exposure, read labels, do not heat anything you intend to ingest in plastic, and bring your own glass to the keg party.

IN THE PAST: Phthalate Blues

Personally, my formal introduction to phthalates was when I quit teaching high school and went to grad school. My research involved isolating and characterizing secondary metabolites in the plant family Rutaceae. The process involved solvent extraction (soxhlet) and evaporation followed by gravitational silica column chromatography. We learned quickly that all the bulk silica, most of the solvents, and the most popular clear flexible tubing (Tygon) all contained di-octylphthalate (DOP), an oil. The air in the building was also loaded with DOP due to the filters. Fortunately, it was easy to keep track of DOP because of its blue fluorescence. The low polarity of the plasticizer made it easy to elute off of the columns with the slurry solvent. For our 20cm x 20cm x 1-2mm thick layer prep plates, we formed and dried them, and then placed them in the chromatography chamber with acetone. Upon re-drying, the plates viewed under UV light were flat white with a bright blue edge along the top.

Most of my targeted metabolites are fluorescent; yellow, green, pink, and blue to the eye. I once inadvertently isolated a non-chromophoric terpene because I was chasing an indigo blue fluorescent spot on the TLC. Upon elution from the plate, I got an oil. Mass spectrometric analysis revealed the terpene in a tableau of DOP fragments. The friend who ran the mass spec for me, Charlie, was in charge of a spectroscopy lab for a veterinary toxicology department at the time. He said he could recognize all the spectrographic manifestations of DOP from twenty paces.

My last encounter with DOP was several years later, in a Pickering customer’s lab. An extremely agitated gentleman had called to announce that he had “NO PEAKS!!!” So, our customer service chemist went for a visit, and I went along for the ride.

We arrived at 10:00am, and fortunately the system was running. He had a Carbamate post-column instrument paired with a water/methanol two-pump, four-piston binary gradient HPLC. The pistons were ganged in series. Our chemist engaged the customer while I observed the instrument. The fluorometer was so overloaded with signal that the PM tube was regularly turning off. There was no troubleshooting information available from the magnitude of the signal, but there was a very regular and periodic spike, implying a piston cycle.

Upon further observation of the HPLC, I noticed that both reservoirs’ contents had traveled up into the Nitrogen lines and was sloshing around in the Tygon tubing. With this back-flowed solution being sloshed back into the reservoir periodically, I realized the problem. Although Tygon tubing is phthalate-free today, it was loaded with DOP back then. The swamping fluorescence was in both reservoirs. The spike frequency was the last piston on the methanol pump, where the DOP concentration would be the highest.

The customer had his peaks, he just couldn’t see them for the bright lights.