• 분석과학
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• 제34권6호
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• pp.241-250
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• 2021

검량선 작성은 기기분석을 통해 생체시료에서 분석물질의 농도를 측정하는 정량분석법 개발과 측정값의 정확도 향상에 있어서 필수적인 요소이다. 본 연구에서는 R 기반 통계분석기법을 이용하여 개별 분석물질 정량에 적합한 가중계수와 회귀모델 선정하기 위한 단계별 선택 기준을 적용하여 분석 프로그램을 설정하였다. 국내에서 남용빈도가 가장 높은 필로폰과 대마 복용여부 확인을 위해 액체크로마토그래피-질량분석법(LC-MS/MS)이 적용되었으며, 분석물질로 마약의 복용 여부를 확인에 일반적으로 사용되는 대상 마약의 모체와 대사체를 소변 시료에서 분석하였다. 검량선 작성에 있어서 가중계수 적용여부는 원본데이터의 이분산성 검정을 통해 확인하였고, 가중계수가 필요하다고 판단된 경우 분산분석을 통해 적정 가중계수를 선정하였다. 다음으로 편분산분석을 이용하여 회귀모델에 적합한 차수를 결정하였다. 분석물질인 메트암페타민, 암페타민, 대마 대사체에 대해 R 기반 프로그램에 적용한 결과, 단계별 결과 및 최종 모델식을 직관적으로 이해하기 쉽고 신속하게 얻을 수 있었다. 이러한 결과는 문서 파일로 저장이 가능하여 보관의 편의성을 제고하였으며, 본 연구를 통해 제작된 R 기반 프로그램을 활용하여 검량선 작성을 필요로 하는 다양한 약물분석 분야에 확대 적용할 수 있을 것으로 판단된다.

• 분석과학
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• 제21권1호
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• pp.41-47
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• 2008

소변 중 암페타민계 5성분(amphetamine; AP, methamphetamine; MA, 3,4-methylenedioxyamphetamine; MDA, 3,4-methylenedioxymethamphetamine; MDMA, 3,4-methylenedioxyethylamphetamine; MDEA)의 동시분석을 위하여 기존의 액체상추출(liquid-liquid extraction; LLE) 방법과는 달리 감정과정의 자동화가 가능한 고체상추출(solid-phase extraction, SPE) 방법을 도입하였다. 시험관에 소변 3 mL와 0.1 M 인산완충액 1 mL (pH 7.0)를 넣고, 자동추출장치를 이용하여 추출하고, 증발 건고하여 유도체화 한 다음 GC/MS로 분석하였다. 그 결과 검정곡선의 직선성 상관계수 ($r^2$)는 AP와 MDA [농도범위 34.0 (AP), 28.0 (MDA)~1000.0 ng/mL] 및 MA, MDMA, MDEA (농도범위 50.0~2000.0 ng/mL)에서 0.994 이상으로 나타났다. 그리고 각 성분들의 검출한계 (LOD)는 4.0~10.0 ng/mL 범위였고, 정량한계 (LOQ)는 12.0~34.0 ng/mL 범위였다. 상대 회수율은 5성분 모두 93.5~107.7%로 측정되었다. 정밀도 (precision)와 정확도 (accuracy)는 각각 1.9~14.8%와 -8.7~14.8 % 범위 값을 나타냈다. 본 실험방법을 실제 남용자 소변에 적용한 결과 메스암페타민 또는 엑스터시 투약자를 신속하고 정확하게 동시에 확인할 수 있었다.

• 약학회지
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• 제55권2호
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• pp.145-153
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• 2011

A simultaneous detection and quantification method for determining the Phenylalkylamine derivatives, such as methamphetamine (MA), amphetamine (AM), 3,4-methylenedioxymethamphetamine (MDMA), 3,4-methylenedioxyamphetamine (MDA), ketamine (KT), norketamine (NKT), phentermine (PT), fenfluramine (FFA) and phenmetrazine (PM), in oral fluid was developed and validated according to international guidelines. The validated method was applied to actual oral fluid samples collected from drug abuse suspects. The recovery of phenylalkylamines from oral fluid collection devices was also assessed. Oral fluid specimens from 20 drug abuse suspects submitted by the police were collected using Salivette$^{TM}$, Quantisal$^{TM}$ or direct expectoration. The samples were screened using a biochip array analyzer. For confirmation, the samples were analyzed by GC-MS in selected-ion monitoring (SIM) mode after extraction using automated SPE with a mixed-mode cation exchange cartridge and derivatization with trifluoroacetic anhydride (TFAA). The results from the immunoassay were consistent with those from GC-MS. All the oral fluid samples gave positive results for MA, AM, PT and/or PM. The detection of phenylalkylamines in oral fluid can provide a better indication of recent use than urine or hair. Therefore, the oral fluid specimen was useful for demonstrating phenylalkylamines abuse in the driving under the influence of drug (DUID) as an alternative specimen for urine.

• 약학회지
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• 제52권2호
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• pp.137-146
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• 2008

Even though driving under the influence of drug (DUID) is a worldwide problem, we, Korea has no regulation system yet except for alcohol, and there are little cases reported related to DUID. In order to investigate the type of abused drugs for drivers in Korea, we tried to analyze controlled and non-controlled drugs in alcohol-positive blood samples. 275 whole bloods, which were positive for alcohol on the roadside test, were collected from the police for two months ($Nov.{\sim}Dec.$ 2006). The analytical strategy was constituted of three steps: First, alcohol in blood samples were confirmed and quantified by gas chromatography. Second, controlled drugs were screened by $Evidence_{investigator}\;^{TM}$ (Randox, U.K.) as preliminary test. It was based on immunoassay by biochip array analyzer. Nine groups of drug abuse were screened: amphetamines, methamphetamines, cannabis, cocaine, opiates, barbiturates, methadone, benzodiazepines I (oxazepam) & II (lorazepam). Finally, confirmation of these drugs was performed by GC-MS. Blood samples were extracted by solid-phase extraction by $RapidTrace^{TM}$ (Zymark, U.S.A.). After trimethylsilyl (TMS) derivatization, eluates were analyzed to GC-MS. Total 49 drugs were investigated in this study including controlled drugs, antidepressants, 1st generation antihistamines, dextromethorphan, nalbuphine, ketamine, etc. For rapid detection, we developed the automated identification system. It was made up a new software, "DrugMan", modified Chemstation data analysis menu and newly developed macro modules. A series of peak selection, identification and reporting of the results were performed automatically by this system. Concentrations of alcohol in 275 blood samples were ranged from 0.011 to 0.249% (average, 0.119%). Among 149 blood samples, just six samples (4.0%) were showed positive results to the immunoassay: one methamphetamine and five benzodiazepines group I. By GC-MS confirmation, only benzodiazepines were detected and methamphetamine was not detected from immunoassay positive blood sample. Besides these drugs, 5 chlorpheniramines, dextromethorphan, diazepam, doxylamine, ibuprofen, lidocaine and topiramate were also detected in whole bloods by GC-MS. Conclusively, the frequency of drug abuse for Korean drivers was relatively low. There was none case which illegal drug was detected. However these results were limited to alcohol positive blood samples, so it is necessary to analyze more samples including alcohol negative blood.