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An accurate and nondestructive GC method for determination of cocaine on US paper currency. Yuegang Zuo Kai Zhang Jingping Wu Christopher Rego John Fritz. Abstract. ∋. 실제 US 지폐의 67% 에서 cocaine 이 검출 . 이는 마약거래 및 마약 복용에 있어 지폐가 이용됨에 따름.

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An accurate and nondestructive GC method for determination of cocaine on US paper currency

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An accurate and nondestructive gc method for determination of cocaine on us paper currency

An accurate and nondestructive GC method for

determination of cocaine on US paper currency

Yuegang Zuo

Kai Zhang

Jingping Wu

Christopher Rego

John Fritz


An accurate and nondestructive gc method for determination of cocaine on us paper currency

Abstract

실제 US 지폐의 67%에서 cocaine이 검출.

이는 마약거래 및 마약 복용에 있어 지폐가 이용됨에 따름.

Pharmaceutical Analysis / S.K.K.U. Dept. of Pharmacy


An accurate and nondestructive gc method for determination of cocaine on us paper currency

What is cocaine?

흰색결정성 알칼로이드.

코카나무(Erythroxylum coca)의 잎에서 추출되는 성분.(C17H21NO4) 신경, 점막자극을 방해

-> 마취제로 사용.

소량 복용 시 식욕감퇴·피로회복·각성효과(쾌감발생).

다량 및 연속적 복용 시 우울증·불안감·자극과민성·수면장애·만성피로·정신혼란·편집증 -> 사망.

3-benzoyloxy-8-methyl-8-azabicyclo[3.2.1]octane-2-carboxylic acid methyl ester

Pharmaceutical Analysis / S.K.K.U. Dept. of Pharmacy


An accurate and nondestructive gc method for determination of cocaine on us paper currency

Introduction

지폐의 코카인 분석이 중요한 이유

: 법의학적 증거 – 용의자 검색

: 유출 route를 파악하기 위한 수단

– 마약 사용의 정성적 데이터 획득

Pharmaceutical Analysis / S.K.K.U. Dept. of Pharmacy


An accurate and nondestructive gc method for determination of cocaine on us paper currency

Material /Methods

US banknote(1,5,10,20,50,100$)

: 실험군 – Southeastern Massachusetts에서 무작위 추출

: 대조군 – American Bank에서 제공

Pharmaceutical Analysis / S.K.K.U. Dept. of Pharmacy


An accurate and nondestructive gc method for determination of cocaine on us paper currency

Material / Methods

Sample extraction and preparation

: 지폐 + 15ml의 물(MeOH) => 20ml의 유리 vial에봉합

=> 실온에서 5분간 초음파 욕조에서 sonicated

: C18 cartridge – 2.00ml의 물 + 2.00ml의 MeOH로 washing.

: 목적시료 – 5.00ml의 MeOH, ethyl acetate, hexane의 혼합물로 eluting.

: Nitrogen, MeOH 475㎕ + internal standard 25㎕ => 500㎕

Pharmaceutical Analysis / S.K.K.U. Dept. of Pharmacy


An accurate and nondestructive gc method for determination of cocaine on us paper currency

Material / Methods

Internal standard

: 내부 표준 물질

: 분석용 검출기에 제시되는 값은 절대적이지 않음

=> 재현성 있는 결과를 주지 못함

: 매 분석 시에 기준을 부여하는 역할

=> 원하는 시료에 대한 상대 값산출 가능

Pharmaceutical Analysis / S.K.K.U. Dept. of Pharmacy


An accurate and nondestructive gc method for determination of cocaine on us paper currency

Material / Methods

VWR, Signature Ultrasonic Cleaner Model 75D, 90W

Pharmaceutical Analysis / S.K.K.U. Dept. of Pharmacy


An accurate and nondestructive gc method for determination of cocaine on us paper currency

Material / Methods

: Shimadzu GC-17A gas chromatograph equipped with a FID 로 수행.

: Injector – Shimadzu AOC-20i GC auto-injector를 사용.

: Data산출 – Gateway E-4200 computer with

CLASS-VP Chromatography Data System Version4.2

: Column – 30 m60.32 mmid, 1.00 lm film ECTM-5 capillary column

: Stationary phase –5% phenyl-polysiloxane 95%

dimethyl-polysiloxane 혼합물

: Carrier Gas – Helium (27cm/s)

FID 검출을 위해 Nitrogen을 보충 가스로 사용.

:Injection – Splitless mode(2㎕)

: Column temperature – 초기 2분간 80℃ 유지

3분간 40℃/min (80℃ ->200℃ ) 4분간 20℃/min(200℃->280℃)

마지막은 3분간 유지

Injector(290℃ 유지), Detector(310℃ 유지)

Pharmaceutical Analysis / S.K.K.U. Dept. of Pharmacy


An accurate and nondestructive gc method for determination of cocaine on us paper currency

Material

: Sample injection method – Liquid sample injection via special microsyringe

: Number of samples – 6 vials

: Syringe speed – 2 Modes(Fast, Slow)

: Plunger speed – 3 Modes(Fast, Medium, Slow)

: Wait time – 0~99 sec following sample aspiration (in 0.1sec steps)

: Type of sample injection – 3 Modes (Traditional, Solvent Flush, Solvent Flush with a Second Solvent)

: Injection volume linearity – ±0.5% (injection volume 1~5 µl, sample n-C12)

Shimadzu AOC-20i GC auto-injector

Pharmaceutical Analysis / S.K.K.U. Dept. of Pharmacy


An accurate and nondestructive gc method for determination of cocaine on us paper currency

Material

Shimadzu GC-17A gas chromatograph equipped with a FID

Pharmaceutical Analysis / S.K.K.U. Dept. of Pharmacy


An accurate and nondestructive gc method for determination of cocaine on us paper currency

Material

Gateway E-4200

CLASS-VP Chromatography Data System Version4.2

Pharmaceutical Analysis / S.K.K.U. Dept. of Pharmacy


An accurate and nondestructive gc method for determination of cocaine on us paper currency

Material

  • Flame Ionization Detector(FID)

    : 가장 널리 사용되는 검출기 중 하나(GC에 일반적 사용)

    : Column의 용출물이 버너에서 수소 및 공기와 혼합되고 전기로 점화, 연소.

    : 버너 끝과 불꽃 위에 위치한 수집 전극 사이에 수백Volts의 전위가 걸려 전류(∼10-12QA)발생 (Impedance 연산증폭기로 측정)

    : 생성 이온 수 ∝ 불꽃에서 환원되는 탄소원자의 수

    : 질량감응장치 – 단위 시간 당 검출기로 유입되는 탄소원자 수에 감응

Pharmaceutical Analysis / S.K.K.U. Dept. of Pharmacy


An accurate and nondestructive gc method for determination of cocaine on us paper currency

Material

: The peak identification, 순도 재확인 – a Hewlett –.Packard (HP) model GC 5890 Series II gas chromatograph coupled with an HP 5971 series mass selective detector and an HP 7673 GC auto sampler로 수행.

: Capillary – DB-5fused-silica capillary column

(30 m60.32 mm id,0.25 lm film, J & W Scientific, Folsom, CA, USA).

: Column temp. – 초기 3분간 80℃ 유지.

그 후 20도℃/min (to 260℃)

: Carrier gas – 3 psi column head pressure/tech oxygen trap사용

: Injector – 280℃ / 1.0㎕의 volume을 splitless mode로 injection.

: Interface temp. – 305℃

Pharmaceutical Analysis / S.K.K.U. Dept. of Pharmacy


An accurate and nondestructive gc method for determination of cocaine on us paper currency

Material

Hewlett –.Packard (HP) model GC 5890 Series II gas chromatograph

Pharmaceutical Analysis / S.K.K.U. Dept. of Pharmacy


An accurate and nondestructive gc method for determination of cocaine on us paper currency

Material

  • Mass spectra:m/z 50 에서 650 까지 1.5 scans/sec. 의 속도로 cocaine검출을 위해 사용.

  • Cocaine으로 의심 되는 피크의 고정시간과 표준 코카인의 피크를 비교하여 수행.

  • Quantification of Cocaine: IS의 피크 면적을 통한 비율에 기초를 두어 수행.

Pharmaceutical Analysis / S.K.K.U. Dept. of Pharmacy


An accurate and nondestructive gc method for determination of cocaine on us paper currency

Results / Discussion

Pharmaceutical Analysis / S.K.K.U. Dept. of Pharmacy


An accurate and nondestructive gc method for determination of cocaine on us paper currency

Results / Discussion

코카인 분리 정량의 용매 결정

: 유기 용매 사용 시 지폐의 손상 및 타 오염물질의 추출

=> 물을 solvent로 활용 – 코카인 확인 방해요소 차단(초음파의 응용)

: Recovery experiment로 물과 MeOH의 추출 효용성 평가

=> 두 solvent 모두 높은 효용성 – 지폐 손상이 없는 물을 선택

Pharmaceutical Analysis / S.K.K.U. Dept. of Pharmacy


An accurate and nondestructive gc method for determination of cocaine on us paper currency

Results / Discussion

Pharmaceutical Analysis / S.K.K.U. Dept. of Pharmacy


An accurate and nondestructive gc method for determination of cocaine on us paper currency

Results / Discussion

Pharmaceutical Analysis / S.K.K.U. Dept. of Pharmacy


An accurate and nondestructive gc method for determination of cocaine on us paper currency

Results / Discussion

Pharmaceutical Analysis / S.K.K.U. Dept. of Pharmacy


An accurate and nondestructive gc method for determination of cocaine on us paper currency

Results / Discussion

Method Validation

: Calibration curve – 0.00~100㎕/ml 사이의 standard solution 사용

– r=0.994, s=1.33×10^-2, i=2.85×10^-3

: LOQ – 지폐 당 4ng으로 설정

: Retention time의 재현성 – 25회의 연속된 injection으로 평가

– 0.02% 미만의 RSD%(높은 재현성)

: Precision of peak area ratio – better than 1.0% (10회의 injection)

Pharmaceutical Analysis / S.K.K.U. Dept. of Pharmacy


An accurate and nondestructive gc method for determination of cocaine on us paper currency

Results / Discussion

검체에따른 분석 결과

: 5, 50달러에선 모두 검출

: 10, 20달러의 대부분에서 검출

: 1, 100달러에선 거의 미검출

=> 모든 지폐에 같은 빈도로 검출되리라는 기존의 가설을 무너뜨림

Pharmaceutical Analysis / S.K.K.U. Dept. of Pharmacy


An accurate and nondestructive gc method for determination of cocaine on us paper currency

Results / Discussion

Further Questions

: # of banknotes – 사용된 지폐의 적은 양이 문제될 수 있음

: Locationfor collecting – Massachusetts 라는 국소적 영역에 국한

: Validation for retention

: Using internal standard(IS) for avoiding influence of circumstance

Pharmaceutical Analysis / S.K.K.U. Dept. of Pharmacy


An accurate and nondestructive gc method for determination of cocaine on us paper currency

References

[1] United Nations Office on Drugs and Crime, 2007 World Drug Report.

[2] ONDCP, What America's Users Spend on Illegal Drugs 1988 – 1995, December 2001, The Office of National Drug Control Policy, Washington, DC.

[3] Aaron, R., Lewis, P., Crime Lab. Digest 1987, 14, 18.

[4] Hudson, J. C., Can. Soc. Forensic Sci. J. 1989, 22, 203 – 219.

[5] Bohannon, J., Science 2007, 316, 42 – 43.

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[7] Jenkins, A. J., Forensic Sci. Int. 2001, 121, 189 – 193.

[8] Negrusz, A., Perry, J. L., Moore, C. M., J. Forensic Sci. 1998, 43, 626 – 629.

[9] Esteve-Turrillas, F. A., Armenta, S., Moros, J., Garrigues, S., Pastor, A., de la Guardia, M., J. Chromatogr. A 2005, 1065, 321 – 325.

[10] Song, D., Zhang, S., Kohlhof, K., J. Chromatogr. A 1996, 731, 355 – 360.

[11] Dixon, S. J., Brereton, R. G., Carter, J. F., Sleeman, R., Anal. Chim. Acta 2006, 559, 54 – 63.

[12] Frederick, K. A., Pertaub, R., Kam, N. W. S., Spectros. Lett. 2004, 37, 301 – 310.

[13] Xu, Y., Gao, Y., Wei, H., Du, Y., Wang, E., J. Chromatogr. A 2006, 1115, 260 – 266.

[14] Keil, A., Talaty, N., Janfelt, C., Noll, R. J., Gao, L., Ouyang, Z., Cooks, R. G., Anal. Chem. 2007, 79, 7734 – 7739.

[15] Zuo, Y., Wang, C., Zhan, J., J. Agric. Food Chem. 2002, 50, 3789 – 3794.

[16] Zuo, Y., Zhang, K., Lin, Y., J. Chromatogr. A 2007, 1148, 211 – 218.

[17] Zuo, Y., Zhang, L., Wu, J., Fritz, J. W., Medeiros, S., Rego, C., Anal. Chim. Acta 2004, 526, 35 – 39.

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[20] Zuo, Y., Wang, C., Lin, Y., Guo, J., Deng, Y., J. Chromatogr. A 2008 in press.

Pharmaceutical Analysis / S.K.K.U. Dept. of Pharmacy


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