S00017052 O O
, GC/MS ph GC/MS I
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
......I Abstract.........V....1 1.1...1 1.1.1 1 1.1.2 1 1.2 GC/MS...2 1.3...3 1.3.1....3 1.3.2 3 1.4... 4 1.4.1... 4 1.4.2......5 1.4.3... 5 1.4.4...6 1.5...7 1.5.1.... 7 1.5.2....8 1.6.....13. 14 2.1. 14 2.1.1....14 2.1.2. 14 2.1.3.....14 2.1.4..... 14 2.1.5. 14 III
2.2........15 2.2.1..... 15 2.2.2......16 2.2.2.1......17 2.2.2.2......18 2.3.... 22 2.4 ph......23 2.5........26 2.6.........26...... 27... 29 GC-MS.... 39......46. 52 1.....53 2......54 3.......55 IV
, 20 amphetamine-type stimulants ATS 21 3000 90 1999 ATS GC/MS ph V
1.1 1.1.1 GC/MS HP5890A HP5970B HP300 HP9153C Sartorius R200D 0.00001g DT-100 0.0001g Galanz WP800 Nichiryo-50 l Nichiryo-200ul -1000 l 10uL,Agilent Technologies LD5-2A Grant instruments TP500 MO-2 Mili-Q SHB XW-80A GL-88B 1.1.2 1.1.2.1 MA 1212-9802 Amp 9301 MDMA 1245-0101
MDA 4- Aldrich chem.co 1.1.2.2 20020318 990615 20000121 990209 20000319 20010816 20020124 1.2 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 250 270 110KPa PFTBA SIM SIM m/z44 86 118 Amp m/z58 100 191 MA m/z58 162 100 MDMA m/z44 162 135 MDA m/z91 191 4-
1.1 min 1 4.00 Amp 44 86 118 2 9.75 MA 58 91 100 3 10.75 4-72 91 191 4 11.85 MDA 44 135 162 5 12.70 MDMA 58 100 162 1.3 1.3.1 (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 1.3.2 4- GC/MS 1.2
1.2 - Rt (min) Rt (min) AMP 5.488 44 65 91 120 9.369 44 86 118 135 MA 6.105 58 65 91 115 10.146 58 100 191 281 7.442 91 45 65 132 11.431 91 191 43 72 MDA 9.093 44 136 77 106 12.290 44 162 135 77 MDMA 9.574 58 135 107 69 13.067 58 162 100 135 Amp MA MDMA MDA 1.4 1.4.1 (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
2 1µl A MA /A i C MA (3) MDMA MA (4) MDA MA 1.4.2 (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 1.4.3 1.4.3.1 (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 1.4.3.2 (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 1.4.4 3 0.5ml
1.5 1.5.1 Amp MA 4- MDMA MDA 9.369 10.146 11.431 12.290 13.067 1.1 1.2 1.3 1.4 1.1 1.2 1.3
1.4 1.5.2 1.5.2.1 (1) Amp Amp 0.025~1.6µg/ml Y = 3.1472X - 0.0557 R 2 = 0.9993 n=2 1.5 3 0.125ng 12.5ng/ml 6 4.5 AAmp/Ai 3 1.5 0 0 0.5 1 1.5 2 ug/ml) 1.5 Amp (2) MA MA 0.05~3.2µg/ml Y = 4.2387X - 0.1068 R 2 = 0.9991 n=2 1.6 3 0.05ng 5ng/ml
16 12 AMA/Ai 8 4 0 0 0.5 1 1.5 2 2.5 3 3.5 ug/ml) 1.6 MA (3) MDMA MDMA 0.05~3.2µg/ml Y = 1.1219X - 0.0484 R 2 = 0.9993 n=2 1.7 3 0.30ng 30ng/ml 4 AMDMA/Ai 3 2 1 0 0 1 2 3 4 ug/ml 1.7 MDMA (4) MDA MDA 0.05~3.2µg/ml Y = 1.9385X - 0.0753 R 2 = 0.9995 n=2 1.8 3 0.25ng 25ng/ml
7.5 6 AMDA/Ai 4.5 3 1.5 0 0 0.5 1 1.5 2 2.5 3 3.5 ug/ml) 1.8 MDA 1.5.2.2 (1) Amp 0.05µg/ml 0.20µg/ml 0.80µg/ml Amp 86.32% 124.73% 1.3 1.3 Amp n=6 µg/ml X ± SD RSD(%) 0.05 119.53 0.06 4.20 0.20 99.34 0.05 4.60 0.80 100.23 4.27 4.26 (2) MA 0.1µg/ml 0.4µg/ml 1.6µg/ml MA 85.33% 119.67% 1.4 1.4 MA n=6 µg/ml X ± SD RSD(%) 0.10 118.06 0.05 3.87 0.40 104.83 0.07 6.40 1.60 95.74 0.09 9.81 - -