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Direct and sensitive analysis of methamphetamine, ketamine, morphine and codeine in human urine by cation-selective exhaustive injection and sweeping micellar electrokinetic chromatography Yi-Hui Lin 1 , Shou-Mei Wu 1,2,3 *. (A). HCB. separation buffer (low pH). stacked cations. (B). EOF.

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  1. Direct and sensitive analysis of methamphetamine, ketamine, morphine and codeine in human urine by cation-selective exhaustive injection and sweeping micellar electrokinetic chromatographyYi-Hui Lin1, Shou-Mei Wu1,2,3* (A) HCB separation buffer (low pH) stacked cations (B) EOF cation analytes sweeping zone (C) EOF micelle buffer (D) EOF No. CE FPIA GC-MS No. CE FPIA GC-MS Drug found Conc. (ng/mL) Drug Found Conc. (ng/mL) Concentration Concentration RSD REa) know found S1 MA >3000 + + S15 MA 4160 + + (ng/mL) (ng/mL) (%) (%) S2 M 2110 + + S16 MA 1601 + + Intra-day analysis (n=3) S3 MA <250 + + S17 M C 1049 285 + + + MA 3.8 x 102 (3.2 ± 0.2) x 102 6.3 -15.8 10.0 x 102 (10.3 ± 0.2) x 102 1.9 3.0 S4 MA <250 + + S18 M 359 + + 3.5 x 103 (3.6 ± 0.1) x 103 2.8 2.9 S5 M C >3000 367 + + + S19 MA >5000 + + K 7.5 x 101 (6.9 ± 0.3) x 101 4.3 -8.0 2.0 x 102 (2.0 ± 0.1) x 102 5.0 0.0 S6 MA <250 + + S20 M 470 + + 7.0 x 102 (6.9 ± 0.1) x 102 1.4 -1.4 S7 MA >5000 + + S21 M >3000 + + C 2.3 x 102 (2.0 ± 0.1) x 102 5.0 -13.0 S8 MA M <250 2015 + + + + S22 MA >5000 + + 6.0 x 102 (6.0 ± 0.1) x 102 1.7 0.0 2.1 x 103 (2.1 ± 0.0) x 103 0.0 0.0 S9 M 404 + + S23 MA 1882 + + M 2.3 x 102 (2.0 ± 0.1) x 102 5.0 -13.0 S10 M 267 + + S24 K 228 ND* + 6.0 x 102 (6.0 ± 0.1) x 102 1.7 0.0 S11 M 435 + + S25 K >1000 ND + 2.1 x 103 (2.1 ± 0.1) x 103 4.8 0.0 S12 MA 2610 + + S26 K >1000 ND + Inter-day analysis (n=5) S13 MA 4649 + + S27 MA K 2663 897 ND + + MA 3.8 x 102 (3.2 ± 0.1) x 102 3.1 -15.8 10.0 x 102 (10.5 ± 0.4) x 102 3.8 5.0 S14 M >3000 + + S28 K >1000 ND + 3.5 x 103 (3.5 ± 0.2) x 103 5.7 0.0 K 7.5 x 101 (7.2 ± 0.3) x 101 4.2 -4.0 2.0 x 102 (2.0 ± 0.1) x 102 5.0 0.0 7.0 x 102 (7.0 ± 0.3) x 102 4.3 0.0 C 2.3 x 102 (2.4 ± 0.2) x 102 8.3 4.3 6.0 x 102 (6.3 ± 0.3) x 102 4.8 5.0 2.1 x 103 (2.0 ± 0.1) x 103 5.0 -4.8 M 2.3 x 102 (2.1 ± 0.2) x 102 9.5 -8.7 6.0 x 102 (6.0 ± 0.3) x 102 5.0 0.0 2.1 x 103 (2.1 ± 0.1) x 103 4.8 0.0 1. Graduate Institute of Pharmaceutical Science, College of Pharmacy, Kaohsiung Medical University, Kaohsiung, Taiwan2. Faculty of Fragrance and Cosmetics, College of Pharmacy, Kaohsiung Medical University, Kaohsiung, Taiwan3. Faculty of Pharmacy, College of Pharmacy, Kaohsiung Medical University, Kaohsiung 807, Taiwan Abstract Cation-selective exhaustive injection and sweeping micellar electrokinetic chromatography (CSEI-Sweep-MEKC) was directly used to test some abuse drugs in human urine, including morphine (M), codeine (C), ketamine (K) and methamphetamine (MA). First, phosphate buffer (50 mM , pH 2.5) containing 30% methanol was filled into uncoated fused silica capillary (40 cm, 50 μm I.D.), then high conductivity buffer (100 mM phosphate, 6.9 kPa for 99.9 s) was followed. Electrokinetic injection (10 kV, 500 s) was used to load samples and to enhance sensitivity. The stacking step and separation were performed at -20 kV and 200 nm using phosphate buffer (25 mM, pH 2.5) containing 20% methanol and 100 mM sodium dodecyl sulfate. Using CSEI-Sweep-MEKC, the analytes could be simultaneously analyzed and have a detection limit down to ppb level. It was unnecessary to have sample pretreatments. During method validation, calibration plots were linear (r≥ 0.9982) over a range of 150 – 3000 ng/mL for M and C, 250 - 5000 ng/mL for MA, and 50 - 1000 ng/mL for K. The limits of detection were 15 ng/mL for M and C, and 5 ng/mL for MA and K (S/N = 3, sampling 500 s at 10 kV). Comparing with capillary zone electrophoresis, the results indicated that this stacking method could increase 6000-fold sensitivity for analysis of MA. Our method was applied for analysis of 28 real urine samples. The results showed good coincidence with immunoassay and GC-MS. This method was feasible for application to detect trace levels of abused drugs in forensic analysis. Figure 2. Scheme of CSEI-Sweep-MEKC mode Results Figure 3. Electropherograms of the standard mixture and three real samples obtained under optimized conditions. Table 1. Precision and accuracy for the determination of MA, K, C and M in urine. Table 2. Data of urine samples from 28 addicts tested by CE, FPIA and GC-MS. *ND, not done. FPIA: fluorescence polarization immunoassay Conclusion The present work provided a potential CSEI-Sweep-MEKC method which could be successfully applied to the direct analysis of urine samples of MA, K, M and C addicts. Figure 1. Structures of MA, K, M and C. * RE (% relative error) = (conc. found – conc. known) x 100/ (conc. known)

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