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Patient Record Systems
An Early
Effort in Street Drug Analysis By James F. Robinson
D
o you sometimes feel that you should use your pharmacy education for something more than counting pills, typing labels and writing prescriptions on a physician's order? I realize that this is an over-simplification of the prescription dispensing process, but there is an ounce of truth in this suggestion, as evidenced by the entrepreneurs among us who expand their interests to include front-end sales and o-t-c advice to the self-medicating patient; and the pharmacist who extends to his patients additional services such as sick -room supplies, support garments, improved labeling and family prescription records. Many pharmacists have found additional use for their knowledge and expertise in community health, public speaking and education on the drug abuse problem confronting our nation. As more and more of our number complement their regular practice with outstanding jobs in these fields, the image of the pharmacist in community affairs becomes increasingly impressive. More important than this is the personal satisfaction of a job well done. A "job well done" may be a premature title to our efforts in Dubuque, Iowa; however, it has given me a chance to use my education in an additional approach to community service. I became involved in drug identification at the Dubuque County Pharmaceutical Association meeting in June 1969 when Capt. Tom Rettenmeier of the Dubuque Police Department addressed the members, introducing the group to some first-hand information on the drug problem in Dubuque. During his talk, Capt. Rettenmeier mentioned that one of the biggest problems the law enforcement officials have is
getting expert testimony in court about the identity of drugs that are picked up in an arrest. After the meeting, I asked him if perhaps we could use some of the chemistry and pharmacognosy learned in pharmacy school to an advantage in the drug identity problem. We agreed that the idea had some merit and met the following day at the Finley Hospital, where I am employed. At this meeting Capt. Rettenmeier provided additional explanation in regard to the drug abuse problem; the time factor seemed to be the big stumbling block to using the state chemistry lab and private laboratories. Frequently, more than two months passed before answers were obtained from these overworked facilities. If we could locally duplicate this process instead of mailing exhibits out of town for analysis, it would facilitate matters considerably. With support from Chief Robert O'Brien of the Dubuque Police Department, we · immediately began gathering information, reference books and equipment. We enlisted the aid of Pedro Vasquez and Carl Osuch of the University of Dubuque chemistry department. They volunteered the use of their infrared and ultraviolet spectrophotometers, and assisted in finding source standards of IR Spectra for 850 drugs. 1 The greatest help has come from Sister Marguerite Neumann, BVM, chairman of the chemistry department at Clarke College of Dubuque. She began working with us early in 1970 and, as a result of her assistance, Clarke College now allows us the use of their modern chemistry laboratory and equipment. This laboratory affords
us the use of IR and UV Spectrophotometers and Gas Chromatograph. Most samples of LSD contain such small quantities (50 to 200 meg) that the use of IR and UV is ruled out, but thinlayer chromatography can be used for f!Ualitative identification. Until the spring of 1970, most of the practical work we were able to accomplish was in testing samples of marijuana and hashish for our own information, at which time Captain Rittenmeier established communications with the Bureau of Narcotics and Dangerous Drugs (BNDD) laboratory in Chicago. From Jerry Nelson, chief chemist, we learned that their laboratory and chemists were available to identify drugs and to assist others in learning the methods which they employ. As a result, I spent three days in the BNDD laboratory in June 1970 as an introduction to forensic chemistry. Sister Marguerite spent three days there in July, and I returned for another session of practical work on a specific problem in the fall. No one can learn to be a forensic chemist in a few days, but by applying their qualitative tests, we learned to identify a small number of the abused drugs. The chemists of the BNDD laboratory in Chicago are some of the finest, most helpful, gentlemen I have had the pleasure of knowing and working with. I have an especially high regard for Jerry Nelson, director of the laboratory and Ferris Van Sickle and David Parmalee, my instructors. During the period from August 1970 through June 1971 , I completed 62 identification tests for court exhibits for the Dubuque Police Department and the Iowa State Highway Patrol, plus several off-the-record tests that Vol. NS13, No. 12, December 1973
677
Inspecting a local specimen ... "Iowa grass."
Extracting a drug sample.
Placing TLC media in Gelman chromatography chamber.
Step two- Duquenois test.
678
Journal of the AMERICAN PHARMACEUTICAL ASSOCIATION
Positive results with the Duquenois test.
were not to be used in court. As an "expert" witness I am apt to be served with a subpoena at any time which will require my appearance before the Grand Jury or on the witness stand in court. Even though this is time-consuming, the results bring a feeling of satisfaction at having done something constructive to aid law enforcement in its fight against the encroachment of illegal drug distribution in our community. Illegality must be avoided in our handling of drugs, also. We are required to be sworn in as special deputies to the sheriff so that we may legally have abuse drugs in our possession. Since marijuana and hashish are the most frequently used drugs presented for identification, I should like to briefly describe the methods employed. By using the Duquenois-Levine test, the official test in the Book of Methods of the Association of Official Analytical Chemists, marijuana can be qualitatively identified without the use of the IR and UV Spectrophotometers and Gas Chromatograph as reported by Nelson and MayThis present study indicates that cannabis plant material can be positively identified by using both the extended Duquenois test and microscopy. Thinlayer chromatography is a valuable confirmatory test, particularly when the sample is hashish and when the presentation of the sample is unusual. 2
This is further confirmed by George R. NakamuraCystolith hairs, important criteria for the identification of marijuana leaf fragments, occur among several dicotyledonous families, notably the Moraceae, Boraginaceae, Loasaceae, Ulmaceae, and Cannaginaceae. Since cysto/iths also develop in many forms, most species can be differentiated from Cannabis only by a very close morphological examination. The Duquenois-Levine test was found useful in confirmation, since none of 82 species, many ofwhich had hairs similar to those found on Cannabis, yielded a positive test. 3
A microscopic examination of the marijuana leaf reveals a warty-appearing top side with numerous cystolith trichomes that resemble bear claws and are typical of the plant. The underside has much longer and more populous trichomes with no cystoliths. The cystoliths on top contain calcium carbonate which, when treated with Werner's Reagent,* will release car-
James F. Robinson practices community pharmacy in Bynum, Alabama. He graduated from Stanford University in Birmingham, Alabama, in 1961 with a BS in pharmacy. In his previous position, he was director ofpharmacy at the Finley Hospital in Dubuque, Iowa. Robinson is past president (1970 and 1971) ofthe Dubuque County Pharmaceutical Association.
bon dioxide gas in a rapid bubbling process. Hashish will frequently yield carbon dioxide and show trichomes even though the morphological structure of the plant has been destroyed in the manufacture of hashish. The second test in identifying marijuana and hashish is the DuquenoisLevine test. At this stage of testing we usually use 25 to 50 milligrams of the sample and extract with petroleum ether (about two milliliters), and then divide into two portions. These portions are placed in evaporating dishes, placed under the hood and evaporated to dryness. Complete dryness is essential because petroleum ether will interfere with the analysis. The constituent that we are interested in extracting for our analysis is tetrahydrocannabinol (THC), the active Ingredient. THC also be extracted from the bowls of pipes that have build-up of THC in the pipe residue. Cigaret papers that are recovered from a partially smoked "joint" have yielded good, positive results. Of the two portions in the evaporating dishes, one will be used for the Duquenois-Levine test and the other for thin-layer chromatography. Proceeding with the former, the extract is dissolved in 2 ml of Duquenois Reagent* placed in a test tube and agitated for one minute; then added to 2 ml concentrated hydrochloric acid and agitated for one minute. If the color of the sample ranges from blue to violet the test is positive; any other color indicates a negative test. There are some other plants that will yield a similar test result to this point: however, the final step will positively identify THC. This final step consists of adding 2 ml of chloroform and agitating for one minute. After allowing the mixture to settle into layers, the lower (chloroform) layer will be a violet to purple color and the upper layer a light blue . The final test for marijuana and hashish is thin-layer chromatography.
*
* Werner's
Reagent: Three parts glacial acetic acid and one part concentrated hydrochloric acid.
Duquenois Reagent: Dissolve 25 drops of acetaldehyde and two grams of vanillin in 700 ml of ethyl alcohol 95 percent and refrigerate. This solution. should be discarded when it becomes discolored.
For this purpose, we have found that Gelman's impregnated glass fiber SA and SAP work best as thin-layer media; benzene for the solvent, and Fast. Blue 2 B* as the developer. Delta 1 and Deltas THC are supplied to us by the BNDD laboratory in Washington, D.C. to use as standards in this test. An extensive method for identifying marijuana by the chromatography method which separates and identifies other components of the plant is described by Dr. R. B. Forney of the Indiana University Medical Center. 4 Another source for identification of nearly all modern pharmaceuticals is Isolation and Identification of Drugs by E.G.C. Clarke. 5 •
*Fast Blue 2 B Powder: This is available from K & K Laboratories in New York City. The solution is one percent in 50 percent methanol.
References 1. 850 Pharmaceutical Infrared Prism Spectra Indices and Spec Finder, Sadder Research Laboratories 2. Nelson, D. F., and May, A. V., "The Identification of Cannabis," UN Secretariat Report (Aug. 15, 1969) 3. Nakamura, G.," Forensic Aspects of Cystolith Hairs of Cannabis and Other Plants," J. of the Assn. of Official Analytical Chem., 52, (Jan. 1969) 4. Turk , R. F., Dharir, H. 1., and Forney, R. B.," A Simple Chemical Method to Identify Marijuana," J. of Forensic Sciences, 14, No.3, 389 5. Clarke, E. G. C., Isolation and Identification of Drugs, Pharmaceutical Press, England (1969)
Bibliography 1. Clarke, E. G. C., Isolation and Identification of Drugs, Pharmaceutical Press, England (1969). Available in the United States from Rittenhouse Book Store, 1706 Rittenhouse Square, Philadelphia, Pa. 2. Nakamura, George, R., "Forensic Aspects of Cystolith Hairs of Cannabis and Other Plants," J. of the Assn. of Official Analytical Chemists, 52, (Jan. 1969) 3. Nelson, D. F. and May, A. V., "The Identification of Cannabis," UN Secretariat Report, (Aug. 15, 1969) 4 . Sadder Research Laboratories, 850 Pharmaceutical Infrared Prism Spectra Indices and Spec Finder, Sad tier Research Laboratories, 3316 Spring Garden Street, Philadelphia, Pa. 5. Turk, R. F., Dharir, H. I., and Forney, R. B., "A Simple Chemical Method to Identify Marijuana," J. of Forensic Sciences, 14, No.3 (1969)
Vol. NS13, No. 12, December 1973
679
Effort in Street Drug Analysis By James F. Robinson
D
o you sometimes feel that you should use your pharmacy education for something more than counting pills, typing labels and writing prescriptions on a physician's order? I realize that this is an over-simplification of the prescription dispensing process, but there is an ounce of truth in this suggestion, as evidenced by the entrepreneurs among us who expand their interests to include front-end sales and o-t-c advice to the self-medicating patient; and the pharmacist who extends to his patients additional services such as sick -room supplies, support garments, improved labeling and family prescription records. Many pharmacists have found additional use for their knowledge and expertise in community health, public speaking and education on the drug abuse problem confronting our nation. As more and more of our number complement their regular practice with outstanding jobs in these fields, the image of the pharmacist in community affairs becomes increasingly impressive. More important than this is the personal satisfaction of a job well done. A "job well done" may be a premature title to our efforts in Dubuque, Iowa; however, it has given me a chance to use my education in an additional approach to community service. I became involved in drug identification at the Dubuque County Pharmaceutical Association meeting in June 1969 when Capt. Tom Rettenmeier of the Dubuque Police Department addressed the members, introducing the group to some first-hand information on the drug problem in Dubuque. During his talk, Capt. Rettenmeier mentioned that one of the biggest problems the law enforcement officials have is
getting expert testimony in court about the identity of drugs that are picked up in an arrest. After the meeting, I asked him if perhaps we could use some of the chemistry and pharmacognosy learned in pharmacy school to an advantage in the drug identity problem. We agreed that the idea had some merit and met the following day at the Finley Hospital, where I am employed. At this meeting Capt. Rettenmeier provided additional explanation in regard to the drug abuse problem; the time factor seemed to be the big stumbling block to using the state chemistry lab and private laboratories. Frequently, more than two months passed before answers were obtained from these overworked facilities. If we could locally duplicate this process instead of mailing exhibits out of town for analysis, it would facilitate matters considerably. With support from Chief Robert O'Brien of the Dubuque Police Department, we · immediately began gathering information, reference books and equipment. We enlisted the aid of Pedro Vasquez and Carl Osuch of the University of Dubuque chemistry department. They volunteered the use of their infrared and ultraviolet spectrophotometers, and assisted in finding source standards of IR Spectra for 850 drugs. 1 The greatest help has come from Sister Marguerite Neumann, BVM, chairman of the chemistry department at Clarke College of Dubuque. She began working with us early in 1970 and, as a result of her assistance, Clarke College now allows us the use of their modern chemistry laboratory and equipment. This laboratory affords
us the use of IR and UV Spectrophotometers and Gas Chromatograph. Most samples of LSD contain such small quantities (50 to 200 meg) that the use of IR and UV is ruled out, but thinlayer chromatography can be used for f!Ualitative identification. Until the spring of 1970, most of the practical work we were able to accomplish was in testing samples of marijuana and hashish for our own information, at which time Captain Rittenmeier established communications with the Bureau of Narcotics and Dangerous Drugs (BNDD) laboratory in Chicago. From Jerry Nelson, chief chemist, we learned that their laboratory and chemists were available to identify drugs and to assist others in learning the methods which they employ. As a result, I spent three days in the BNDD laboratory in June 1970 as an introduction to forensic chemistry. Sister Marguerite spent three days there in July, and I returned for another session of practical work on a specific problem in the fall. No one can learn to be a forensic chemist in a few days, but by applying their qualitative tests, we learned to identify a small number of the abused drugs. The chemists of the BNDD laboratory in Chicago are some of the finest, most helpful, gentlemen I have had the pleasure of knowing and working with. I have an especially high regard for Jerry Nelson, director of the laboratory and Ferris Van Sickle and David Parmalee, my instructors. During the period from August 1970 through June 1971 , I completed 62 identification tests for court exhibits for the Dubuque Police Department and the Iowa State Highway Patrol, plus several off-the-record tests that Vol. NS13, No. 12, December 1973
677
Inspecting a local specimen ... "Iowa grass."
Extracting a drug sample.
Placing TLC media in Gelman chromatography chamber.
Step two- Duquenois test.
678
Journal of the AMERICAN PHARMACEUTICAL ASSOCIATION
Positive results with the Duquenois test.
were not to be used in court. As an "expert" witness I am apt to be served with a subpoena at any time which will require my appearance before the Grand Jury or on the witness stand in court. Even though this is time-consuming, the results bring a feeling of satisfaction at having done something constructive to aid law enforcement in its fight against the encroachment of illegal drug distribution in our community. Illegality must be avoided in our handling of drugs, also. We are required to be sworn in as special deputies to the sheriff so that we may legally have abuse drugs in our possession. Since marijuana and hashish are the most frequently used drugs presented for identification, I should like to briefly describe the methods employed. By using the Duquenois-Levine test, the official test in the Book of Methods of the Association of Official Analytical Chemists, marijuana can be qualitatively identified without the use of the IR and UV Spectrophotometers and Gas Chromatograph as reported by Nelson and MayThis present study indicates that cannabis plant material can be positively identified by using both the extended Duquenois test and microscopy. Thinlayer chromatography is a valuable confirmatory test, particularly when the sample is hashish and when the presentation of the sample is unusual. 2
This is further confirmed by George R. NakamuraCystolith hairs, important criteria for the identification of marijuana leaf fragments, occur among several dicotyledonous families, notably the Moraceae, Boraginaceae, Loasaceae, Ulmaceae, and Cannaginaceae. Since cysto/iths also develop in many forms, most species can be differentiated from Cannabis only by a very close morphological examination. The Duquenois-Levine test was found useful in confirmation, since none of 82 species, many ofwhich had hairs similar to those found on Cannabis, yielded a positive test. 3
A microscopic examination of the marijuana leaf reveals a warty-appearing top side with numerous cystolith trichomes that resemble bear claws and are typical of the plant. The underside has much longer and more populous trichomes with no cystoliths. The cystoliths on top contain calcium carbonate which, when treated with Werner's Reagent,* will release car-
James F. Robinson practices community pharmacy in Bynum, Alabama. He graduated from Stanford University in Birmingham, Alabama, in 1961 with a BS in pharmacy. In his previous position, he was director ofpharmacy at the Finley Hospital in Dubuque, Iowa. Robinson is past president (1970 and 1971) ofthe Dubuque County Pharmaceutical Association.
bon dioxide gas in a rapid bubbling process. Hashish will frequently yield carbon dioxide and show trichomes even though the morphological structure of the plant has been destroyed in the manufacture of hashish. The second test in identifying marijuana and hashish is the DuquenoisLevine test. At this stage of testing we usually use 25 to 50 milligrams of the sample and extract with petroleum ether (about two milliliters), and then divide into two portions. These portions are placed in evaporating dishes, placed under the hood and evaporated to dryness. Complete dryness is essential because petroleum ether will interfere with the analysis. The constituent that we are interested in extracting for our analysis is tetrahydrocannabinol (THC), the active Ingredient. THC also be extracted from the bowls of pipes that have build-up of THC in the pipe residue. Cigaret papers that are recovered from a partially smoked "joint" have yielded good, positive results. Of the two portions in the evaporating dishes, one will be used for the Duquenois-Levine test and the other for thin-layer chromatography. Proceeding with the former, the extract is dissolved in 2 ml of Duquenois Reagent* placed in a test tube and agitated for one minute; then added to 2 ml concentrated hydrochloric acid and agitated for one minute. If the color of the sample ranges from blue to violet the test is positive; any other color indicates a negative test. There are some other plants that will yield a similar test result to this point: however, the final step will positively identify THC. This final step consists of adding 2 ml of chloroform and agitating for one minute. After allowing the mixture to settle into layers, the lower (chloroform) layer will be a violet to purple color and the upper layer a light blue . The final test for marijuana and hashish is thin-layer chromatography.
*
* Werner's
Reagent: Three parts glacial acetic acid and one part concentrated hydrochloric acid.
Duquenois Reagent: Dissolve 25 drops of acetaldehyde and two grams of vanillin in 700 ml of ethyl alcohol 95 percent and refrigerate. This solution. should be discarded when it becomes discolored.
For this purpose, we have found that Gelman's impregnated glass fiber SA and SAP work best as thin-layer media; benzene for the solvent, and Fast. Blue 2 B* as the developer. Delta 1 and Deltas THC are supplied to us by the BNDD laboratory in Washington, D.C. to use as standards in this test. An extensive method for identifying marijuana by the chromatography method which separates and identifies other components of the plant is described by Dr. R. B. Forney of the Indiana University Medical Center. 4 Another source for identification of nearly all modern pharmaceuticals is Isolation and Identification of Drugs by E.G.C. Clarke. 5 •
*Fast Blue 2 B Powder: This is available from K & K Laboratories in New York City. The solution is one percent in 50 percent methanol.
References 1. 850 Pharmaceutical Infrared Prism Spectra Indices and Spec Finder, Sadder Research Laboratories 2. Nelson, D. F., and May, A. V., "The Identification of Cannabis," UN Secretariat Report (Aug. 15, 1969) 3. Nakamura, G.," Forensic Aspects of Cystolith Hairs of Cannabis and Other Plants," J. of the Assn. of Official Analytical Chem., 52, (Jan. 1969) 4. Turk , R. F., Dharir, H. 1., and Forney, R. B.," A Simple Chemical Method to Identify Marijuana," J. of Forensic Sciences, 14, No.3, 389 5. Clarke, E. G. C., Isolation and Identification of Drugs, Pharmaceutical Press, England (1969)
Bibliography 1. Clarke, E. G. C., Isolation and Identification of Drugs, Pharmaceutical Press, England (1969). Available in the United States from Rittenhouse Book Store, 1706 Rittenhouse Square, Philadelphia, Pa. 2. Nakamura, George, R., "Forensic Aspects of Cystolith Hairs of Cannabis and Other Plants," J. of the Assn. of Official Analytical Chemists, 52, (Jan. 1969) 3. Nelson, D. F. and May, A. V., "The Identification of Cannabis," UN Secretariat Report, (Aug. 15, 1969) 4 . Sadder Research Laboratories, 850 Pharmaceutical Infrared Prism Spectra Indices and Spec Finder, Sad tier Research Laboratories, 3316 Spring Garden Street, Philadelphia, Pa. 5. Turk, R. F., Dharir, H. I., and Forney, R. B., "A Simple Chemical Method to Identify Marijuana," J. of Forensic Sciences, 14, No.3 (1969)
Vol. NS13, No. 12, December 1973
679