Department of Pharmaceutical Analysis, School of Pharmacy, Hebei Medical University, Shijiazhuang, Hebei Province 050017, China.
Procuratoral Technology and Information Research Center, Supreme People's Procuratorate, Beijing 100144, China.
J Chromatogr B Analyt Technol Biomed Life Sci. 2014 Apr 1;955-956:10-9. doi: 10.1016/j.jchromb.2014.02.007. Epub 2014 Feb 18.
A rapid and sensitive method based on solid phase extraction and ultra performance liquid chromatography-electrospray ionization tandem mass spectrometry (UPLC-ESI-MS/MS) for the simultaneous determination of amphetamine, methamphetamine, 3,4-methylenedioxyamphetamine, 3,4-methylene-dioxymethamphetamine, N-methyl-1-(3,4-methyl-enedioxyphenyl)-2-butanamine, 3,4-methylenedioxyethylamphetamine, p-methoxymethamphetamine, ephedrine, N-methylephedrine, cathinone, methcathinone, and ketamine in whole blood and urine was developed and validated. Following solid phase extraction, the analytes were separated on ACQUITY UPLC BEH Phenyl column (100mm×2.1mm, 1.7μm) under gradient elution using a mobile phase containing of acetonitrile and 0.3% formic acid in water at a flow rate of 0.4mLmin(-1) and analyzed by a triplequadrupole mass spectrometer in the multiple reaction monitoring (MRM) mode. The proposed method was linear for each analyte with correlation coefficients over 0.99. Recovery validation studies showed accuracy bias below 4.4%. Acceptable precision was also obtained with a relative standard deviation below 8.9%. The sensitivity of the assay was found to be adequate for the quantitation of the illicit drugs in whole blood and urine sample and was higher than reported methods. The present method was proved to be reliable and robust for drug screening in forensic toxicological analysis.
基于固相萃取和超高效液相色谱-电喷雾串联质谱(UPLC-ESI-MS/MS)的快速灵敏方法,用于同时测定全血和尿液中的苯丙胺、甲基苯丙胺、3,4-亚甲二氧基苯丙胺、3,4-亚甲二氧基甲基苯丙胺、N-甲基-1-(3,4-亚甲二氧苯基)-2-丁胺、3,4-亚甲二氧基乙基苯丙胺、对甲氧基苯丙胺、麻黄碱、N-甲基麻黄碱、卡西酮、甲卡西酮和氯胺酮。固相萃取后,采用含乙腈和 0.3%甲酸的水作为流动相,在 ACQUITY UPLC BEH Phenyl 柱(100mm×2.1mm,1.7μm)上进行梯度洗脱,流速为 0.4mLmin(-1),在三重四极杆质谱仪上以多反应监测(MRM)模式进行分析。该方法对每种分析物均呈线性,相关系数均大于 0.99。回收率验证研究表明,准确度偏差低于 4.4%。相对标准偏差也低于 8.9%,可获得良好的精密度。该方法的灵敏度足以定量全血和尿液中的非法药物,且灵敏度高于已报道的方法。该方法在法医毒理学分析中的药物筛选中被证明是可靠和稳健的。