, GC/MS ph GC/MS I

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3 Abstract Drug abuse is a serious issue throughout the world. Amphetamine-type stimulants (ATS) are substances frequently used by drug abusers. There are significant needs to develop a quick and accurate analytical method for detection of ATS in suspicious urine samples. In the present study, a novel GC-MS method was developed that allows simultaneous detection of four amphetamine derivatives, which has not been reported previously in literature. The four classes of amphetamine have been quantified using the same extraction and chromatographic conditions. The data were analyzed statistically. The method developed has been successfully applied in quantitation of amphetamine species in the urine samples collected from suspects located in different regions, Beijing and Wuhan. The results indicate that: 1) The chemical compositions in suspicious urine can be classified, and the concentrations of amphetamine species can be obtained using the current method. Therefore, a threshold for determination of drug abuse can be established based on the data. Furthermore, the results can be used in developing the index of a drug abusing testing box. 2) The relationship between the urine ph values and amphetamine concentration was revealed for the first time in literature. In conclusion, a simple and quick analytical method was developed for assay of amphetamine derivatives in urine samples and the experimental results provide valuable information for future development of quick and accurate monitoring methods of the ATS abuse. Key words GC/MS Amphetamines Quantitative analysis Urine sample II

4 ......I Abstract V GC/MS III

5 ph GC-MS IV

6 , 20 amphetamine-type stimulants ATS ATS GC/MS ph V

7 GC/MS HP5890A HP5970B HP300 HP9153C Sartorius R200D g DT g Galanz WP800 Nichiryo-50 l Nichiryo-200ul l 10uL,Agilent Technologies LD5-2A Grant instruments TP500 MO-2 Mili-Q SHB XW-80A GL-88B MA Amp 9301 MDMA

8 MDA 4- Aldrich chem.co GC/MS - 4- GC/MS GC HP-5 25 m 0.12 mm 0.33 m 4min 80 1min 15 /min 245 2min 14min MS EI 70 ev 2200V KPa PFTBA SIM SIM m/z Amp m/z MA m/z MDMA m/z MDA m/z

9 1.1 min Amp MA MDA MDMA (1) Amp MA MDMA MDA (2) 20ng/ l 4-50 l 1 g 0.5ml (3) 5% NaOH ph >11 NaCl 1.0ml 2min 3600rpm 12 min (4) 5ml 50 l 100 l Galanz 2-3min (5) N 2 (6) 50 l 1 l GC/MS 1.2

10 1.2 - Rt (min) Rt (min) AMP MA MDA MDMA Amp MA MDMA MDA (1) Amp 4- i Amp 4-2µg Amp 0.025µg 0.05µg 0.1µg 0.2µg 0.4µg 0.8µg 1.6µg 2 1µl A Amp /A i C Amp (2) MA 4- i MA 4-2µg MA 0.05µg 0.1µg 0.2µg 0.4µg 0.8µg 1.6µg 3.2µg

11 2 1µl A MA /A i C MA (3) MDMA MA (4) MDA MA (1) Amp 0.05µg 0.2µg 0.8µg/ml Amp Amp 6 (2) MA 0.1µg 0.4µg 1.6µg/ml MA MA 6 (3) MDMA MA (4) MDA MA (1) Amp 0.05µg 0.2µg 0.8µg/ml Amp

12 Amp 6 (2) MA 0.1µg 0.4µg 1.6µg/ml MA MA 6 (3) MDMA MA (4) MDA MA (1) Amp 0.05µg 0.2µg 0.8µg/ml Amp Amp 1 6 (2) MA 0.1µg 0.4µg 1.6µg/ml MA MA 1 6 (3) MDMA MA (4) MDA MA ml

13 Amp MA 4- MDMA MDA

14 (1) Amp Amp 0.025~1.6µg/ml Y = X R 2 = n= ng 12.5ng/ml AAmp/Ai ug/ml) 1.5 Amp (2) MA MA 0.05~3.2µg/ml Y = X R 2 = n= ng 5ng/ml

15 16 12 AMA/Ai ug/ml) 1.6 MA (3) MDMA MDMA 0.05~3.2µg/ml Y = X R 2 = n= ng 30ng/ml 4 AMDMA/Ai ug/ml 1.7 MDMA (4) MDA MDA 0.05~3.2µg/ml Y = X R 2 = n= ng 25ng/ml

16 7.5 6 AMDA/Ai ug/ml) 1.8 MDA (1) Amp 0.05µg/ml 0.20µg/ml 0.80µg/ml Amp 86.32% % Amp n=6 µg/ml X ± SD RSD(%) (2) MA 0.1µg/ml 0.4µg/ml 1.6µg/ml MA 85.33% % MA n=6 µg/ml X ± SD RSD(%)

Microsoft Word - 4期中文目次.doc

Microsoft Word - 4期中文目次.doc 中草药 Chinese Traditional and Herbal Drugs 第 45 卷第 4 期 2014 年 2 月 509 UPLC-MS/MS 法快速检测减肥类保健品中 13 种非法添加化学成分朱健, 裘一婧, 沈国芳杭州市食品药品检验研究院, 浙江杭州 310017 摘要 : 目的建立保