Lin Yi-Hui, Lee Maw-Rong, Lee Ren-Jye, Ko Wei-Kung, Wu Shou-Mei
Graduate Institute of Pharmaceutical Science, College of Pharmacy, Kaohsiung Medical University, Kaohsiung, Taiwan.
J Chromatogr A. 2007 Mar 23;1145(1-2):234-40. doi: 10.1016/j.chroma.2007.01.054. Epub 2007 Jan 18.
We established a capillary electrophoretic method with high sensitivity and specificity for testing hair taken from addicts. After pretreatment of hair sample, the cation-selective exhaustive injection and sweeping micellar electrokinetic chromatography (CSEI-Sweep-MEKC) was used to test for the presence of abused drugs in human hair. These drugs include morphine (M), codeine (C), ketamine (K) and methamphetamine (MA). First, an uncoated fused-silica capillary (40 cm, 50 microm I.D.) was filled with phosphate buffer (50 mM, pH 2.5) containing 30% methanol, followed by high conductivity buffer (100 mM phosphate, 6.9 kPa for 99.9 s). Electrokinetic injection (10 kV, 600 s) was used to load samples and to enhance sensitivity. Stacking steps and separations were performed at -20 kV with detection at 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 the level of picogram per milligram hair. During method validation, calibration plots were linear (r > or = 0.999) over a range of 0.15-80 ng/mg hair for MA and K, 0.3-30 ng/mg hair for C and 0.5-50 ng/mg hair for M. The limits of detection were 50 pg/mg hair for MA and K, 100 pg/mg hair for C and 200 pg/mg hair for M (S/N=3, sampling 600 s at 10 kV). Our method was applied for analysis of real hair samples taken from addicts. The addicts' specimens were also analyzed by LC-MS, and showed good coincidence of results. This method has proven feasible for application in detecting trace levels of abused drugs in forensic analysis.
我们建立了一种用于检测吸毒者头发的具有高灵敏度和特异性的毛细管电泳方法。对头发样本进行预处理后,采用阳离子选择性完全进样和扫集胶束电动色谱法(CSEI-Sweep-MEKC)检测人发中滥用药物的存在情况。这些药物包括吗啡(M)、可待因(C)、氯胺酮(K)和甲基苯丙胺(MA)。首先,将一根未涂层熔融石英毛细管(40 cm,内径50μm)填充含30%甲醇的磷酸盐缓冲液(50 mM,pH 2.5),接着填充高电导率缓冲液(100 mM磷酸盐,6.9 kPa,99.9 s)。采用电动进样(10 kV,600 s)加载样品并提高灵敏度。在 -20 kV下进行堆积步骤和分离,检测波长为200 nm,使用含20%甲醇和100 mM十二烷基硫酸钠的磷酸盐缓冲液(25 mM,pH 2.5)。使用CSEI-Sweep-MEKC,可同时分析分析物,检测限低至每毫克头发皮克级别。在方法验证过程中,校准曲线在MA和K为0.15 - 80 ng/mg头发、C为0.3 - 30 ng/mg头发、M为0.5 - 50 ng/mg头发的范围内呈线性(r≥0.999)。MA和K的检测限为50 pg/mg头发,C为100 pg/mg头发,M为200 pg/mg头发(S/N = 3,10 kV下采样600 s)。我们的方法应用于分析从吸毒者处采集的实际头发样本。吸毒者的样本也通过液相色谱 - 质谱联用仪进行了分析,结果显示出良好的一致性。该方法已被证明可用于法医分析中检测痕量滥用药物。