Headspace-SPME-GC-MS에 의한 생체시료 중 암페타민계 각성제의 동시분석법 개발
A validated analytical method for simultaneous detection of amphetamine-type stimulants in human urine using HS-SPME-GC-MS
The fluorescence polarization immunoassay (FPIA) as a preliminary test sometimes gives false positive results due to structural similarity between amphetamine-type stimulants (ATS). Thus, a rapid and easy HS (headspace)-SPME (solid-phase microextraction)-GC (gas chromatography)-MS (mass spectrometry) screening method was developed and validated for simultaneous detection of 8 ATS in human urine. These drugs include methamphetamine, amphetamine, MDMA (3,4-methylenedioxymethamphetamine) and MDA (3,4-methylenedioxyamphetamine) which are popular abused drugs and their metabolites in Korea. Phentermine, ephedrine, pseudoephedrine and norephedrine/norpseudoephedrine also show cross- reactivity by FPIA. The conditions of SPME extraction time, temperature and deposition time were optimized to yield the highest peak area. To prevent carryover, the fiber was baked out pre and post injection into GC/MS. The data was collected by extracted ion chromatogram for each drug from total ion chromatograms by full scan mode and calculated by peak area ratios. Amphetamine, methamphetamine, MDA, MDMA and phentermine showed good resolution with retention times, whereas ephedrine, pseudoephedrine and norephedrine/norpesudo-ephedrine were not detected up to 1 μg/mL. The calibration curve showed acceptable linearity for each drug with R2> 0.99. The results of the intra-and inter-day precision and accuracy were satisfactory: <15 % for precision and within ±10 % for accuracy at three different concentrations (0.167, 0.333, 1.00 μg/mL). Thus, HS-SPME-GC-MS has the advantages of an easy sample preparation with acceptable accuracy and precision for the simultaneous quantification. It will be a useful method for a simple and rapid screening analysis of urines for ATS abuse.
목차
Abstract Ⅰ. 서론 Ⅱ. 재료 및 방법 1. 시약 및 재료 2. 표준 시료의 조제 3. Headspace-SPME 및 GC/MS 조건 4. 암페타민류 약물의 GC/MS에 의한 확인시험 Ⅲ. 결과 및 고찰 1. 암페타민류 각성제에 대한 분석조건 확립 2. 시험방법의 유효화 3. 실제 소변에서 암페타민계 각성제의 분석 Ⅳ. 참고문헌
법과학 분야는 사회정의 구현에 있어 크나큰 가치가 있음에도 불구하고 우리나라에서는 이 분야에 대한 인식이 미흡하여 선진 외국에 비해 침체되어 있는 실정이다. 이에 우리나라에서도 법과학 분야와 관련 있는 학계, 연구기관, 수사기관 등 유관 단체들로 구성된 한국 법과학회를 창립하여 이 분야를 활성화 시켜 과학수사를 한층 더 발전시키기 위함을 목적으로 한다.