Tests for nutraceutical products

The use of herbal preparations in the United States is growing. According to a report prepared by the Beverage Marketing Corp. of New York, approximately 60 million Americans now regularly consume herbal preparations. Nearly 11 million took ginkgo biloba extract, 7.5 million took St. John’s wort and 7.3 million took echinacea in 1997. According to Food Technology’s own Liz Sloan, in a Top Ten Trends article in the August 1999 issue, vitamin and herbal sales topped $12 billion in the past year.

Herbs fall into a regulatory twilight zone. Seasonings and flavors have been safely consumed for centuries, and herbs have also been used for medicinal purposes throughout recorded history in the many ancient cultures. The pertinent regulatory question is: should herbal extracts be regulated as foods or drugs?

Herbal specifications, quality standards, and dosages are important considerations for the food industry and regulatory agencies. Deaths have occurred because products have not been standardized. In 1997, the Food and Drug Administration proposed to limit the amount of ephedrine alkaloids in dietary supplements (e.g., ephedra, ma huang, Chinese ephedra, and epitonin) and require warning labels. An herbal ingredient, plantain, was withdrawn from the market because it was contaminated with another botanical. Cases of kidney failure and cancer resulted when the Arisolochia was accidentally substituted for the herb Stephania.

In the United States, herbs are regulated as dietary supplements along with vitamins, minerals, and amino acids. FDA has authority to regulate questionable herbal health claims, under the Dietary Supplement Health and Education Act of 1994 (DSHEA).

The United States Pharmacopeia (USP) is an organization that establishes standards for drugs, nutritional supplements, medical devices, and equipment. USP standards are well recognized by government agencies and are enforceable by the FDA. USP began focusing on herbs and botanicals in 1996. USP decided that appropriate standards must be developed for herbs to ensure product quality. Information must be available for consumers to assure safe use. Identification tests, analytical methods, information sources, claims, and potential health risk issues are included in the standards. Since 1996, USP has been developing separate monographs on herbs.

An important quality and safety standard for herbs is the analysis for pesticide residues. Analysis of herbs for pesticide residues requires very specialized analytical methods. Positive results, when detected in a small percentage of samples, must always be confirmed by further tests to eliminate any possibility of experimental error. Gas-liquid chromatography is the major technique used to separate the various residue compounds. High-pressure liquid chromatography (HPLC) is an alternative technique. Besides its use for pesticide residue analysis, HPLC is widely used in the analysis of other compounds. In the food laboratory, the technique can be used for vitamin analysis; separation, detection, and profiling of juice components; analysis of aflatoxins in milk; amino acid determination in baby foods; and many other applications.

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As an example of the HPLC technique and its use in the analysis of herbal extracts, at the 1999 IFT Annual Meeting and Food Expo, R. Lenoble of Hauser, Inc., presented a paper on the standardization of nutraceutical products tested with HPLC. The HPLC assays for St. John’s wort (Hypericum perforatum) and echinacea (mainly Echinacea purpurea and Echinacea angustifolia) focused on phenolic compounds. Phenolics are ideally suited for chromatography because of their polarity, solubility, and absorption of UV light. In contrast, the numerous marker compounds found in ginseng (Panax ginseng and Panax quinquefolius) are triterpene saponins and often lead to a complicated chromatogram. The marker compounds for kava kava (Piper methysticum) are aromatic kavalactones and chromatograph easily. The Evaporative Light Scattering Detector (ELSD) was also used with HPLC to detect the triterpene glycosides found in black cohosh (Cimicifuga racemosa).

Chromatography techniques may also be used to isolate antioxidant compounds from spices such as rosemary, and the Rancimat method may be used to test their antioxidant activity. 

Another useful technique for analysis of herbs and spices is the use of chemical sensor arrays or electronic noses. For the study of spices and herbs, electronic nose analytical results can be compared to gas chromatographic analyses of the volatile oil fractions. Researchers have found significant correlations between the electronic nose analyses of cinnamon and rosemary and descriptive sensory analyses. 

The United States Pharmacopeia may be contacted at 12601 Twinbrook Parkway, Rockville, MD 20852 (phone 800-822-8772; www.usp.org).

PATENTS
Method and compositions to detect autooxidation of lipids or fats ex vivo. U.S. patent 5,945,295, filed 12/22/1997, issued 8/31/1999 to J. Roberts et. al., assigned to Vanderbilt University and Lipoprotein Diagnostics, Inc. Describes a method to assess food spoilage ex vivo by quantification of prostanoid compounds and their metabolites produced by a non-cyclooxygenase free radical catalyzed mechanism.

Method and apparatus for using image analysis to determine meat and carcass characteristics. U.S. patent 5,944,598, filed 8/19/1997, issued 8/31/1999 to A. Tong et. al., assigned to Agri-Food Canada. Describes a process and apparatus for determining grading parameters of a carcass. In the process, an outline of an image of the carcass is traced, and reference points representing anatomical features of the carcass are identified. Other measurements which can be obtained from the carcass image and used as independent variables in predictive equations include distances from dorsal and ventral regions of the carcass image outline to a carcass mid-line, carcass widths, angular measurements between reference points, and measurements of curvature of the carcass image outline.

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Products & Literature
CAPILLARY ELECTROPHORESIS SYSTEMS, called the P/ACETM Series, are featured in a quarterly newsletter featuring manuscripts on CE applications, tips on operating conditions, literature highlights, details on upcoming scientific meetings, and information on new instruments. For more information or a copy of the current newsletter, contact Beckman Coulter, Inc., 4300 N. Harbor Blvd., Fullerton, CA 92835 (phone 714-871-4848; fax 714-773-8283; www.beckmancoulter.com) —or circle xxx.

HOT HAND WARNING LABELS may be used to identify hot objects and help to prevent injury. Telatemp Corp. is offering trial samples of the Hot Hand Indicator, a product designed to prevent burn injury to personnel from accidental contact with dangerously hot surfaces. The bright-yellow adhesive label appears blank when cold, but when the surface temperature to which the label is adhered exceeds 50°C, the word “hot” and a warning graphic of a burning hand appears. The labels can be used over the range of –30 to 90°C in environments where ultraviolet exposure is not excessive. Possible applications include electric motors, gas and diesel engines, pumps, valves, furnaces, boilers, ovens, stream pipes, and water heaters—any surface that could radiate extreme heat. For more information, contact Telatemp Corp., 351 Raymond Ave., Fullerton, CA 92831-4624 (phone 714-879-2901; fax 714-870-8136; www.telatemp.com) —or circle ssss.

THERMOGRAVIMETRIC ANALYZER, the Pyris™ 1, may be used for the analysis of moisture content with respect to packaging properties and shelf-life studies. The analyzer also can identify the country of origin of nuts, frostings, spreads of all types, snack foods, and dairy products. The instrument features a built-in balance and furnace. An autosampler may be set to run up to 20 samples. Additional features of the instrument include alloy and quartz hangdown wires that ensure precision; a balance on top, isolated from the furnace; cool-down from 1,000 to 40^oC in less than 15 min for increased sample throughput; and a segmented furnace for quick cleanup. For more information, contact Perkin-Elmer LLC, 761 Main Ave., Norwalk, CT 06859-0237 (phone 800-762-4000; fax 203-762-2812)—or circle xxx.

COLORIMETERS may be used for the objective color measurement of food products such as oils, fats, and syrups. The Lovibond PFX880/L expresses color in terms of red, yellow, and blue, and neutral units that make up the Lovibond Color scale. The Lovibond PFX880/AT gives color data according to the AOCSTintometer Color scale, a special red and yellow version of the Lovibond scale. Chlorophyll A&B and beta-carotene measurements are also available for both instruments with the addition of an upgrade kit. Both instruments feature a long sample chamber for cells up to a 6-in path length. For more information, contact Tintometer Ltd., The Color Laboratory, Waterloo Rd., Salisbury, SP1 2JY, UK (phone 44-1722-327242; fax 44-1722-412322)—or circle xxx.

MINI-POCKET BALANCE, the CRD-150, allows the user to take a balance into the field for checkweighing, sample gathering, and preparation. The balance measures 90 mm × 62 mm × 8 mm with a platform size of 55 mm × 62 mm and weighs in g, oz, dwt, and oz. The weighing capacity is 150 g. Additional features include auto-off function after 4 min of no activity and over- and under-load indicators. The balance runs on two button cell batteries. For more information, contact Markson Lab Scales, 5285 NE Elam Young Pkwy., Suite A-400, Hillsboro, OR 97124 (phone 800-528-5114; fax 800-858-2243)—or circle xxx.

MULTIPOINT MONITOR, the MP100, may be used to monitor multiple instruments simultaneously from one PC. The unit can connect up to eight instruments to one PC with up to nine of the units the user can create a network of 64 instruments. Each instrument can be placed up to 1,000 ft away from the unit, making remote monitoring possible. For more information, contact Dickson Co., 930 S. Westwood Ave., Addison, IL 60101-4997 (phone 630-563-230)—or circle sss. 

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Beer and Wine
REGULATORY OVERVIEW
The following information is part of a series of that provides an overview of the international and U.S. regulatory requirements for a variety of food commodities. This month’s installment is on the regulatory and analytical testing requirements for beer and wine. This information has been supplied by Perkin-Elmer’s food and beverage team. Perkin-Elmer supplies analytical laboratory instruments to perform a variety of tests. For more information, contact The Perkin-Elmer Corp., 761 Main Ave., Norwalk, CT 06859-0010 (phone 800-762-4000 ext. 2522; fax 203-761-2812; e-mail foodbeverage@perkin-elmer; www.perkin-elmer.com). 

Every part of wine and beer production and marketing is regulated in the U.S. Wineries and breweries before beginning any procedure must meet all requirements of Title 27 of the Code of Federal Regulations. These regulations are enforced by the Bureau of Alcohol, Tobacco, and Firearms (ATF), which is a part of the U.S. Treasury Dept. They dictate not only label compliance and matters relating to taxation, which are of interest to consumers, but contain all of the details of permitted processes for, and additions to, wines. They assure identity and authenticity of the product to prevent unfair or fraudulent practices, which is to the benefit of the consumer and the conscientious producer. The BATF regulations are not identical to those for other countries, but the U.S. generally allows the import of wines made legally in other countries as long as they are properly labeled and healthfulness has not been compromised. The reverse is often not the case. 

U.S. LAW
The proof of distilled spirits shall be determined by the use of gauging instruments. hydrometers and thermometers, as prescribed in 27 CFR 30.21. Proprietors and ATF officers shall use only accurate precision-grade hydrometers and thermometers that show subdivisions or graduations of proof and temperature as described in 27 CFR 30.22. The director may authorize ATF officers to use other instruments approved by the director as being equally satisfactory for the determination of specific gravity (SpG) and for gauging. ATF officers shall verify the accuracy of hydrometers and thermometers from time to time. 

A gallon of liquid at 60°F which contains 50% by volume of EtOH having a SpG of 0.7939 at 60°F (referred to water at 60°F as unity), or the alcoholic content thereof is referred to as a proof gallon. Taxation is based on proof. 

According to 27 CFR 77.22, a brand label must have the brand name; class name and address (unless it is branded into the bottle); net contents (unless it is branded into the bottle); name and address of the importer if pertinent (may be on a separate label on the front or back); and the name and address of the bottler or processor if pertinent; and percent alcohol by volume (if required by state law). 

According to 27 CFR 7, H7.71, malt beverages containing 0.5% or more content shall be reported to nearest 0.1%, less than 0.5% content shall be reported to nearest 0.01%. Malt beverages containing 0.5% or more shall have a tolerance of 0.3% in either direction of the stated value. Any beverage labeled as containing 0.5% or more alcohol by volume may not contain less than 0.5% regardless of tolerance. “Low or Reduced Alcohol” beverages must contain less than 2.5% ABV regardless of any tolerances. For beverages containing less than 0.5% ABV, the content cannot exceed the labeled alcoholic content regardless of tolerances. 

“Non Alcoholic Beverages” may be used on beverages but must contain the statement “contains less than 0.5% (or .5%) alcohol by volume in direct conjunction with the term “nonalcoholic.” “Alcohol Free” may be used only on malt beverages containing no alcohol. The terms %OG or %OE may be labeled (unless prohibited by state law). FD&C Yellow No. 5 must be declared for anything bottled after 10/6/84. Saccharin must be labeled. Sulfites must be declared. Aspartame must be declared on anything bottled after 7/9/87 (or any approved label after 1/9/87) or any samples pulled after 1/9/88. 

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There are many regulations concerning the taxation of beer. The 27 CFR 25 describes measurement requirements that pertain to the volume of beer dispensed. 27 CFR 30 contains the gauging manual of distilled spirits requirements. 

Occasionally, ATF circulates rulings which find their origin in other organizations, such as AOAC (Association of Official Analytical Chemists), or OIV (Office International de la Vigne et du Vin {France}). ATF sends these rulings directly to manufacturers. One example of this would be that sulfur dioxide in wine greater than 10 ppm must be labeled. The current U.S. law allows a larger percentage to be present. 

FDA is responsible for some regulations such as contamination in wine. However, the Wine Institute still uses BATF methods and does not have its own methods for regulation. 

ATF permits no more acetic acid than 1.4 g/L in red table wine, and 1.2 g/L in white and dessert wines; California and the European Union, slightly less. California requires a minimum fixed acidity as tartaric of 4.0 g/L for red table, 3.0 g/L for white table, and 2.5 g/L for dessert wines. California also requires a minimum extract in dry wines of 18 g/L for red, and 17 g/L for white. Other states generally do not specify a minimum. In the U.S., maximum total sulfur dioxide is 350 mg/L. Far less is usually used today in wines. European limits are lower for dry wines and higher for sweet table wines. Regulations specify a considerable list of additives that may be permitted under controlled limits and conditions. It is important to note that no wine receives more than a few of these treatments and many have none. An example is that grape musts ferment readily without additions, but some extra nitrogen source for the yeasts is sometimes helpful. If additional nitrogen is necessary, ammonium phosphate is the most commonly used. 

Accurate records must be kept to enable proof of compliance. Each lot of wine must be traceable back to the grapes and vineyards. Tanks must be carefully gauged and the total content recorded on them. If the wine is to be labeled “estate bottled,” the wine must be fermented, processed, and bottled by the state winery at its listed address, and the vineyard must also be owned or controlled by the same winery. Other label terminology is important such as: “produced,” i.e., fermented 75% or made into a different class of wine; “vinted,” “cellared,” or “prepared,” i.e., subjected to cellar processing or aging without changing the class of wine; “blended,” i.e., combined at the state address, wines, probably purchased, of the same class and type, and “bottled” or “packed” by the stated winery. 

EUROPEAN REGULATIONS
Alcohol is the only component monitored for regulatory compliance due to the taxation status. In the UK, the Standard Reference Method is distillation. Other methods, through use, have attained the Recommended Method Status. Generally, government inspectors accept that the method produces results comparable to distillation. There is no formal protocol for attaining the Recommended Method Status, but typically this occurs when enough instruments are in laboratories to adequately establish that the technique is comparable, reliable, repeatable, accurate, and robust. IOB (Institute of Brewing—big in UK only), EBC (European Brewing Congress—for all of Europe), and ASBC (American Society of Brewing Chemists) would likely be involved with the work.

by JAMES GIESE
Associate Editor