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March 2008 Edition
Office of Indiana State Chemist and Seed Commissioner Newsletter
 
Newsletter Contents:
Office of Indiana State Chemist Laboratories - Overview
Microbiology Laboratory
Fertilizer/Trace/Proximate Laboratory Section
Drugs and Vitamins Laboratory Section
Pesticide Formulation Laboratory
Pesticide Residue Laboratory Section
Contact Us
 
Office of Indiana State Chemist - An Overview
Rodney J. Noel,
Ph.D., Lab Director/Associate State Chemist
     
  The Indiana State Chemist Laboratory functions in support of the enforcement of the state laws that the Office of Indiana State Chemist administers. This started in 1881 with the creation of this office which resulted in the analysis of commercial fertilizers in an effort to assure purchasers that they were receiving the proper grade of fertilizer. Over the years, there have been additional laws added to the responsibility of the Indiana State Chemist. This has required additional laboratory analyses, staff and equipment.

The laboratory is divided into five different sections, with a supervisor for each section. There is the Pesticide Residue Section which analyzes samples in support of the Indiana Pesticide Use and Application Law (IC 15-3-3.6). The Microbiology Section supports both the Indiana Commercial Feed Law (IC-15-5-13) and the Indiana Pesticide Registration Law (IC 15-3-3.5). The Pesticide Formulation Section analyzes pesticide products that are required to be registered in the State of Indiana under the Indiana Pesticide Registration Law. The Fertilizer and Automated Analysis Section supports administration of the Indiana Commercial Fertilizer Law (15-3-3-1) and the Indiana Commercial Feed Law. The last section is the Animal Feed Drug and Vitamin Section, which supports the Indiana Commercial Feed Law.

The laboratories are staffed by 24 full-time professional chemists and microbiologists. The support staff includes two half-time technicians, a sample preparation technician and an administrative assistant. In addition, several students are hired throughout the year to aid the chemists in the laboratory.

Many of the analyses performed in the State Chemist Laboratory require highly sophisticated instrumentation. Our laboratory has taken great pride in maintaining a cutting-edge approach to the analysis of the products. Our laboratory staff is well-trained and participates in several organizations such as AOAC International. Our philosophy is to utilize the best possible methods and procedures available for all analyses done in the Indiana State Chemist Laboratory.

If you have any questions regarding the laboratories, please contact:

Dr. Rodney J. Noel
Telephone: (765) 494-5900
E-mail: noelr@purdue.edu
 
     
 
 
Microbiology Laboratory
H.S. Ragheb, Ph.D., Microbiology Supervisor
     
  The Microbiology Department at Indiana State Chemist laboratories began the examination of antibiotics in feeds in 1962. At that time the Indiana State Chemist was Dr. Forest Quackenbush who was also the Head of Biochemistry Department at Purdue University. At first, feed samples were examined for their antibiotic content to enforce the State Commercial Feed Law as well as to participate in collaborative studies with the Association of Official Analytical Chemists (AOAC). The activities were mainly those initiated and conducted by the Food and Drug Administration, which is responsible not only for food safety but also for feed stuffs. As time progressed the number of feed samples examined increased. The samples were complete feeds as well as premixes.

The microbiological analysis of antibiotics in feeds is not an easy task. The technique is complex and requires special attention to details by the analysts. Variability in results within and between laboratories resulted in lack of confidence in analytical results. To address this issue in May 1970, Dr. E.D. Schall the Indiana State Chemist convened a symposium at Purdue University. The discussion on each antibiotic was led by each AOAC Associate Referee. These were scientists employed by the pharmaceutical companies who manufacture these antibiotics. Dr. W.W. Wright from FDA’s Center of Antibiotics Analysis, also the AOAC General Referee on antibiotics in feeds, participated throughout the symposium and coordinated many discussions. Participants who represented 40 laboratories were involved in day to day discussion of the assay techniques and problems. The symposium was cosponsored by the Association of Official Analytical Chemists, the Association of American Feed Control Officials, and the Office of Indiana State Chemist, Purdue University. The proceedings of the symposium were later published and distributed to all participants. The symposium was the forerunner of the current AOAC Forum for Antibiotics and Drugs in Feeds.

Throughout its operation, the Microbiology Laboratory has participated in every AOAC collaborative study on antibiotic analysis in feeds. The Laboratory also initiated and completed two studies on chlortetracycline and bacitracin assay. As a result one method for analysis of chlortetracycline by the turbidimetric method was approved by AOAC as Official Final Action in 1996. The laboratory staff has participated in analytical research and method development. Over 20 manuscripts were published on these topics. The laboratory developed the bioautograph techniques for detecting residue of monensin and other antibiotics in feeds. Such feeds are usually accidentally contaminated and may result in death of animals. For many years the laboratory monitored the good food manufacturing practices (GMP) of feed samples collected by Indiana State Chemist Inspectors. Not only the presence of an antibiotic was determined but also samples were checked for drug combinations.

In 1990, the supervisor of the laboratory was appointed by AOAC as General Referee for antibiotics in feeds. As time passed, the laboratory has developed an excellent reputation and confidence among the feed and pharmaceutical manufacturers. On many occasions, outside laboratories sent samples to the State Chemist Microbiology Laboratory for analysis. These samples are usually "problematic" because of interference by feed components and lower level of antibiotic fortification.

Other activities of the Microbiology Laboratory include the examination of the bacterial and yeast load inoculants. For a short period of time the laboratory was involved with EPA in determining disinfectant efficacy and sporocidal testing. Currently, many more varieties of antibiotics are analyzed. For example, in 1999, the number of feed samples examined for antibiotics content were 226. The antibiotics tested included apramycin, bacitracin, bambermycin, chlortetracycline, hygromycin, lincomycin, oxytetracycline, penicillin, monensin, neomycin, salinomycin, tylosin and virginiamycin. The analysis of these compounds in feeds is relevant especially for those who advocate the control of the use of antimicrobials in animals and their impact on foodborne pathogens.
 
     
 
 
Fertilizer/Trace/Proximate Laboratory Section
James Bartos, Section Supervisor
     
  This section of the laboratory has 6 employees, analysts Sally Mullins, Natalie Newlon, Patricia Waller, and Irene Szalasny, half-time assistant Connie Lehe, and supervisor James Bartos. During the spring and fall seasons of the year, the focus is on fertilizer analysis. At these times, when fertilizer is actively being sold in the marketplace, our inspectors will collect 3000 to 3500 samples of fertilizer products. The remainder of the year is devoted to the analysis of animal feeds, and our inspectors will again collect 3000 to 3500 animal feed samples.

The chemists are responsible for analysis of nitrogen, phosphorus, potassium, sulfur, and micronutrients (trace metal elements) in fertilizers. Additionally, each fertilizer season a number of fertilizer samples are screened for lead, cadmium, and other heavy metals. In the area of animal feeds, the section is responsible for the analysis of protein, calcium, phosphorus, micronutrients, selenium, chromium, and other non nutritive trace elements, and for proximate analysis (moisture, fat, fiber, ash, etc.).

Since the analytical responsibilities of the Section include many of the most commonly guaranteed components of these agricultural products, the workload is high volume, batch oriented. The Section employs a number of quite specialized automated instruments, is highly computerized, and relies heavily on statistical quality control of analytical results. And since the primary emphasis in the regulatory context is accuracy, it is policy that no sample is reported as being deficient relative to product guarantee, unless it has be analyzed at least twice, on two separate days, with good agreement between individual results.

In addition to the routine workload, the chemists devote a substantial amount of time to development of new methods, and refinement of existing methods. The laboratory actively participates in AOAC International, a professional association for analytical chemists, in the development of standardized and validated chemical methodology, which can be demonstrated to perform well in the hands of different chemists, in independent laboratories.
 
     
 
 
Drugs and Vitamins Laboratory Section
Victoria Siegel, Ph.D., Section Supervisor
     
  The Drugs and Vitamins Laboratory Section at OISC is responsible for analyzing animal feeds and feed ingredients to determine levels of drugs, vitamins, mycotoxins, and other components. Drugs are assayed at the premix, feeding, and residue levels and include the antibacterials not determined by microbiological methods, antimicrobials, coccidiostats, and anthelmintics. Other feed components assayed include amino acids, lactose, sugars, fats, and enzymes. This section also screens animal feeds for the presence of prohibited bovine materials.

Feed components are determined mostly using high performance liquid chromatography, although spectrophotometric, titrimetric, molecular techniques and gravimetric methods are also used. The staff for this section includes five full-time B.S. or M.S. analytical chemists and one section supervisor.
The section supervisor is Chair of the Association of American Feed Control Officials Collaborative Check Sample Program.  This program currently has over 300 enrolled participants from all over the world, and provides a monthly test sample to allow laboratories to monitor the performance of their lab analysts and analytical methods.
 
     
 
 
Pesticide Formulation Laboratory
Ping Wan, Section Supervisor
     
  Since the early 1950’s the pesticide formulation laboratory section at OISC has been analyzing commercial pesticide products in support of state and federal pesticide laws. The laboratory performs chemical assays on products to confirm label claims for active ingredients and is also involved in label review. Each product brought in is maintained in strict chain-of-custody, documented using digital photography and is analyzed for the chemical active ingredient. Many products contain more than one active ingredient and each individual component is reviewed. Pesticide products come in many different forms. While the majority of products can be classified as solid or liquid, there are many different matrices within these main categories. Liquids can be micro-encapsulated, packaged as aerosols, in trigger sprays or impregnated onto towels or wipes. Solids can be gels, ointment, dusts, granules, small pellets, large tablets or pet collars. Each individual product is sampled so that a representative test portion is analyzed.

It is the goal of the laboratory to perform high quality analysis of pesticide products to accurately determine whether they meet the requirements of label claim. The data generated by the laboratory must be legally defensible and every effort is taken to ensure that it stands up in court. The laboratory strives to maintain a broad range of capability and is in contact with pesticide manufacturers to obtain methods for new active ingredients and improved methods for existing products. Equipment is maintained well and up-dated as necessary, making use of available funding through a cooperative agreement with EPA.

Since 2000, the pesticide formulation laboratory at OISC was recognized by our regional branch of EPA and has been designated as the official EPA Region 5 Backup Laboratory. The laboratory performs assays for enforcement samples collected by the EPA regional pesticide investigators; and also supports the Region 5 state formulation laboratories with their needs of sample analysis, data reviewing and methods development.

The laboratory also operates the AAPCO (Association of American Pesticide Control Officials) Check Sample Program, which is a proficiency testing program open to labs conducting both regulatory and commercial pesticide analyses. The aim of the program is to maintain the quality of analytical work and to increase the analytical capability of the participant laboratories. The current membership involves 70 domestic and international labs, from 38 U.S. states and countries all over the world.
 
     
 
 
Pesticide Residue Laboratory Section
Jeff Hardy, Section Supervisor
     
  The Office of Indiana State Chemist Pesticide Residue Laboratory has a laboratory supervisor, three full time analytical chemists and a part time lab technician.  Two basic sample types are analyzed by the residue laboratory: "for cause" investigative residue samples and water samples.

The "for cause" samples range in matrices from soil to plant material to sneakers to children’s toys and everything in between. The laboratory uses state of the art equipment to analyze these samples for trace amount of pesticides. The laboratory uses methods established by the manufacturer, EPA, FDA, AOAC International, and in-house fully validated methods.

Water samples including groundwater and surface water are analyzed semi-routinely by the residue lab for pesticide residues.  Recently the laboratory has also developed the capability to analyze for important pesticide degredates and metabolites in water samples.

The integrity of the samples, maintenance of a strict chain of custody and rigorous quality control is very important for each sample received by the pesticide residue laboratory.
 
     
 
 
Contact Us
     
 

If you have any comments about the newsletter or have any questions about our office, please contact us at:

Office of Indiana State Chemist
Purdue University
175 S. University Street
West Lafayette, IN 47907-2063
Telephone: 765-494-1492
Fax: 765-494-4331

Editor:  Melinda Walsh