Over the years, many allegations have been presented by individuals involved in the clandestine manufacture of amphetamine and methamphetamine centering on the extraction of essential precursors or actual controlled substances from common commercial products. Two such allegations involved the extraction of phenyl-2-propanone, a precursor in the manufacture of amphetamine and methamphetamine, from pesticides, herbicides or photographic chemicals. A third allegation from suspected laboratory operators and confidential informants claimed that amphetamine, methamphetamine and their precursors could be extracted from chicken laying meal. An investigation into these allegations is presented.
Background
As with many different facets of society, the drug culture is not without its myths, legends and old wives' tales that seem to perpetuate over the years from older, more experienced users to the newer, inexperienced users. How such folklore begins is not known, neither is the source nor the reasoning behind the offering of such lore as fact.
The clandestine drug laboratory situation in the United States has been steadily worsening since 1980, with methamphetamine leading as the type of drug most commonly manufactured illegally. To combat the problem, the Federal government and many state governments have sponsored specialized investigative task forces to deal specifically with the investigation, detection, seizure and prosecution of individuals engaged in the manufacture and trafficking of clandestinely produced drugs. These task force agents are police officers with a general understanding of the chemistry applied to the common routes of synthesis of amphetamine, methamphetamine and phencyclidine. However, when information outside their personal knowledge is obtained, the agents turn to a forensic chemist to provide answers as to the feasibility of a particular method. In the past few years, several different "myths" have surfaced concerning the possible diversion of everyday common and legally possessed items for use as precursors in clandestine amphetamine or methamphetamine laboratories.
One myth centres on the extraction of liquid pesticides, herbicides or fertilizers to obtain phenethylamine precursors (Manchester R, personal communication). While these products contain aromatic amines, some fairly complex in structure, they are present in such small quantities as to discourage serious consideration for diversion. Most of these liquid products contain less than 1% of the active ingredient, with the balance being an inert vehicle for easy dilution in water.
Another myth suggests that precursors such as phenyl-2-propanone (P-2-P) are present in common photographic chemistry products and can be extracted from the solutions for use in clandestine synthesis. Most colour film and print developers, black and white film and paper developers and colour reversal film developers contain substituted phenolic amine salts, other amines such as ethylenediamine and hydroxylamine, benzyl alcohol and formaldehyde1. It is possible that at one time a clandestine chemist looked up the structures of these compounds in the Merck Index2, noticed the aromatic moiety and the hydroxyl groups, and hypothesised that they might be chemically altered to produce some raw materials needed for phenethylamine synthesis. However, the quantity of these phenolic and phenolic amine compounds present are low, as working solutions of the developers are approximately 1% in aqueous solution. This myth surfaced again about 1982 in the San Diego, California area when a research chemist for Eastman Kodak (Rochester, New York) was contacted concerning the claim (Abercrombie T, personal communication). Luckily, this chemist had a forensic background and was familiar with most of the common routes and precursors for phenethylamine synthesis. A search of Kodak's records for the previous 15 years, and a literature search back another 10 years failed to show any precursor materials being used in Kodak's photographic chemical formulations.
Interestingly, P-2-P was used in a commercial glass and plastic cleaner called Opti-Kleen (Industrial Optical Service, Pembroke, Massachusetts). Its use in the product pre-dated the scheduling of P-2-P as a controlled substance under Federal law. The Drug Enforcement Administration granted Industrial Optical Service an exemption (the only exemption to date) under the provisions of 21 CFR 130823, allowing them to continue using P-2-P in Opti-Kleen. The concentration of P-2-P in the cleaning product was less than 2% and represented a use of 40kg of P-2-P during the year 1981. However, because of the stringent Federal registration, record keeping and accountability, the company stopped using P-2-P in its formulation of Opti-Kleen in 1982 (Dal Cason T, Sottolano S, Murphy J, personal communications).
The focus of the present paper is an intriguing myth that has been in circulation since the middle 1960s (Hall, C, personal communication). This story has it that since the late 1950s, feed companies have mixed stimulants such as amphetamine, methamphetamine and/or ephedrine into the laying meal feed for chickens. The addition of the stimulant was supposed to help increase the egg output of the hens. It is not uncommon occasionally to run across a known violator purchasing, or in possession of, several hundred pounds of laying meal, probably with the intent to extract the stimulants chemically. In a recent Federal trial in Sacramento, California, the defendant maintained he had purchased and possessed a large quantity of ephedrine to feed to his chickens (Simpson N, personal communication). Another suspected clandestine chemist attempted to purchase large quantities of ephedrine for chicken feed from a chemical supplier in Salt Lake City, Utah (Filmore C, personal communication). A third suspected clandestine chemist justified his possession of nearly 250 pounds (113 kg) of ephedrine as being "...like an antibiotic..." for hogs when mixed 1 part in 10 with hog feed (Freelove D, personal communication). l-Ephedrine has an oral LD50 in mice of 400 mg/kg2.
What might give more credence to this particular myth is the fact that at least seven handwritten recipes or procedures have been collected by the author from suspected violators over the past 4 to 6 years. This suggested that there might be something to it. The motivation behind this investigation came as a result of a late Friday afternoon inquiry from detectives from the Yellowstone County Sheriff's Office in Billings, Montana. The detectives were, in fact, sceptical of the process, yet found solvents, buckets and a 100 pound (45 kg) bag of laying meal in a suspect's garage. Copies of the procedures from this incident, along with copies of other procedures seized in the areas near Riverside, Fresno, and Sacramento, California (Abercrombie T, Massetti J and Michaels C, respectively, personal communications) were examined and an investigation launched into the recent history of chicken laying meal formulation.
Investigation
Laying meal is a complex mixture of crude protein, fat, fibre and minerals, especially calcium. The obvious nature of the feed is to provide a high protein food source to allow a great laying capacity, while providing important minerals like calcium to produce hard egg shells. A typical list of ingredients includes ground corn; soybean, meat and bone meal; corn gluten meal, dehydrated alfalfa meal, vitamins A, D3, E and B12, folic acid, and a high calcium source, such as oyster shell. The feeds generally come in two types, 16 and 20, that describe the percentage of calcium present, and are usually a part of the product name.
The investigation involved three phases: checking with the US Food and Drug Administration (FDA); determining the historical and current background on the formulation of laying meal from several manufacturers; and following the seized procedures on a sample of the laying meal and chemically examining the extract for phenethylamine compounds or precursors.
The FDA is the regulating agency of the Federal government that recommends and approves industry standards for a wide range of products, including food stuffs, drugs and cosmetics. The FDA is also responsible for monitoring compliance with those standards through chemical analysis of materials. Employees of the FDA, involved during the late 1960s and early 1970s with approving feed formulations, were polled to determine if the use of stimulants, specifically phenethylamines, was ever approved for use in laying meal or any other type of livestock feed products. It was found that stimulants had never been approved by FDA for use in those products (McCormick, A, personal communication).
Three major manufacturers of livestock feed products were contacted concerning the history of the production of their feeds and the current formulation of their laying meal. Nutrena (Stockton, CA), a division of Cargill Corporation, indicated that no stimulants were added to their feeds Layer 16, and Layer 20. Occasionally, an antibiotic might be added to some of their feeds targeted at broilers. The common drug used is Amprolium (Amprol-25), and it is added to prevent coccidiosis, a disease in chickens caused by fungi of the genus Coccidioides that may be parasitic in humans. This drug is approved for use in the feeds by FDA (Gomez D, personal communication). The poultry division of Ralston-Purina (St Louis, MO Layenna) also confirmed no stimulants had ever been added to their laying meals, nor were they presently being added. They did indicate, much like Nutrena, that antibiotics or other FDA approved medications might be mixed with the feeds (Engsten H, personal communication).
Manna Pro Corporation (Los Angeles, CA-Egg Maker 16, Egg Maker 20) indicated that no stimulants had ever been added to laying meals produced by Manna Pro, or the previous companies. Manna Pro was originally the Albers Feed Company, and was subsequently sold to Carnation and Nestle's before finally becoming Manna Pro. This issue was raised with retired members of the technical staff and none could remember the addition of any stimulants to the feed. Quite the contrary, it seems that stress and hysteria are two problems that must be monitored in the layers. In the early days (dates unknown) it was common for Albers to put reserpine, a sedative, into the feeds to treat the hysteria (Aydin A, personal communication). One of the products that Manna Pro, and originally Albers, is known for is Calf Manna. This is a higher quality protein feed designed to be used with calves shortly after weaning. The feed also contains anisole, oats and oat meal, and some herbs, and is known to relieve stress in livestock. While it was designed for use with calves, it is widely used as an additive and supplement feed for cattle, horses (show and race) and other show-type livestock. Manna Pro did indicate that Calf Manna had been mixed into laying meal formulated for sale in Japan. Interestingly, Manna Pro receives inquiries from university level athletes concerning the ingredients of the Calf Manna product. It is not known whether the athletes are trying to determine if the feed contains steroids that might promote growth in the calves (and, thus, could be used to enhance their performance), or if the feed can be used as a high protein food supplement.
The handwritten procedures detailing the extraction of the chicken laying meal obtained during investigations were examined. All were similar in content, with the major difference being that two of them required gentle heat to remove the excess solvent. This similarity is interesting, considering the broad geographical distance from their points of collection. The procedures, which included hand-drawn diagrams of equipment set-ups, similar to notes seized in most clandestine drug laboratories, can be generalised as follows:
- The laying meal is placed in a large container, such as a five-gallon (20 litre) plastic or metal bucket.
- Methanol, acetone, or a mixture of both, is added to the meal and is soaked for four to six hours. The liquid is decanted from the meal through large filter papers or through several layers of cheese-cloth into another bucket.
- The solvent is evaporated at ambient temperature with a fan or by gentle heating on a stove or hot-plate. The residue is then dried and used.
- One recipe suggested placing the residue in cookie sheets and spraying it with ethyl ether, then drying in an oven until hard like a brick, breaking it into chunks, and sifting with a final cut of vitamin B12 or Vita-Blend. This recipe reported an approximate yield of 16 to 20 pounds (7.2-9.0 kg) of material from a 100 pound (45 kg) sack of feed.
Experimental
Nutrena Layer 16 (40 g) was ground in a mortar and soaked in methanol/ acetone (1:1) for 6 hours. The solvent was vac vacuum filtered, collected and removed by gentle heating on a hot water bath. A viscous, green-coloured syrup was recovered. This residue was washed with petroleum ether, which removed most of the green coloration. The petroleum ether-insoluble material was isolated and dissolved in a minimal amount of chloroform/ methanol (4:1). If a water-soluble salt of a phenethylamine were present in the meal, it would be soluble in this solvent mixture.
This residue was examined by capillary gas chromatography-mass spectrometry (Hewlett Packard Model 58987) using a 12.5 m x 0.20 mm cross-linked 5% methylphenyl silicone (0.33 micron film thickness) column. A temperature program starting at 100°C for 2 minutes, ramping at 15° per minute to a final temperature of 300°C for 2 minutes was used. These same conditions are used to examine suspected clandestine phenethylamine evidence for precursors, reaction by-products and finished product.
Figure 2 shows the total ion (TIC) of the extract. Two major peaks were noted at 9.16 and 1032 minutes. A library search of the first gave a hit of hexadecanoic acid (palmitic acid), commonly found in oils and fats. The second peak also gave a library search return of low confidence of several long-chain carboxylic acids. Other fatty acids identified in the extract were pentadecanoic acid, the methyl ether of oleic acid and the ethyl ester of hexadecanoic acid. This was not surprising since this laying meal contains a minimum of 3% crude fat by weight. The petroleum ether wash was examined and found to be rich in fatty acids.
The primary area of interest of the TIC is the region from about 2.0 to 5.0 minutes, where the phenethylamines and their precursors commonly elute during routine examination. A library search to identify the peaks at 3.15 and 3.48 minutes was unsuccessful. However, these two compounds clearly were not of the phenethylamine class. Both mass spectra lacked the familiar m/z 91 and 77 ions, typical of mono-substituted benzene rings and did not exhibit base peaks of m/z 44, 58 or 72 representing the beta cleavage of the amine in phenylpropanolamine, amphetamine, ephedrine, methamphetamine, methylephedrine or dimethylamphetamine. The spectra did, however, exhibit the typical "picket fence" appearance of long chain hydrocarbons with obvious losses of m/z 14 and 28 in several places.
Conclusion
The myth of chicken laying meals containing stimulants such as amphetamine or methamphetamine which can be diverted and extracted by clandestine drug laboratory operators is laid to rest. The myth was disproved by an investigation on three independent fronts including the Food and Drug Administration; interviews with three major manufacturers of laying meals on the historical and current trends in meal formulations; and by the chemical examination of an extract obtained by using seized clandestine notes.
