CAJ | 학술논문

目的：建立人体全血中4-溴-2,5-二甲氧基苯乙胺的衍生化 GC/MS 分析方法。方法血液样品经去离子水稀释4倍，8000r/min 高速离心20min 后，加入 NaH2PO4缓冲溶液（pH 值为6.0）2mL，混匀。将上述混合液加入用甲醇、NaH2PO4缓冲溶液（pH 值为6.0）活化的 Bond Elut Centify?固相萃取柱后，依次采用1.0M乙酸溶液、去离子水、甲醇、二氯甲烷/异丙醇/氨水（78/20/2，V/V/V）混合洗脱液进行提取、分离、净化处理，40℃空气流下挥干，三氟乙酸酐衍生化，GC/MS 检测4-溴-2,5-二甲氧基苯乙胺和4-苯基丁胺衍生物。采用标准品衍生化产物的标准质谱图定性分析，选择 m/z 242（4-溴-2,5-二甲氧基苯乙胺）、m/z 91（4-苯基丁胺）作为定量离子进行定量分析。结果血液中4-溴-2,5-二甲氧基苯乙胺的最低检出限为6ng/mL，在0.02~10μg/mL 浓度范围内，线性关系良好（=0.9993），日内精密度和日间精密度均小于10%，平均提取回收率约为69%。结论该方法操作简便、灵敏度高，适用于全血中4-溴-2,5-二甲氧基苯乙胺检测。
목적：건립인체전혈중4-추-2,5-이갑양기분을알적연생화 GC/MS 분석방법。방법혈액양품경거리자수희석4배，8000r/min 고속리심20min 후，가입 NaH2PO4완충용액（pH 치위6.0）2mL，혼균。장상술혼합액가입용갑순、NaH2PO4완충용액（pH 치위6.0）활화적 Bond Elut Centify?고상췌취주후，의차채용1.0M을산용액、거리자수、갑순、이록갑완/이병순/안수（78/20/2，V/V/V）혼합세탈액진행제취、분리、정화처리，40℃공기류하휘간，삼불을산항연생화，GC/MS 검측4-추-2,5-이갑양기분을알화4-분기정알연생물。채용표준품연생화산물적표준질보도정성분석，선택 m/z 242（4-추-2,5-이갑양기분을알）、m/z 91（4-분기정알）작위정량리자진행정량분석。결과혈액중4-추-2,5-이갑양기분을알적최저검출한위6ng/mL，재0.02~10μg/mL 농도범위내，선성관계량호（=0.9993），일내정밀도화일간정밀도균소우10%，평균제취회수솔약위69%。결론해방법조작간편、령민도고，괄용우전혈중4-추-2,5-이갑양기분을알검측。
Objective To establish a GC/MS derivatization method for determining the 4-bromo-2, 5-dimethoxy-phenethylamine in blood. Methods Blood sample was extracted and purified by Bond Elut Centify? solid phase extraction column after diluted to four times by deionized water. The residuum was derivatized by trifluoroacetic anhydride. 4-bromo-2, 5-dimethoxyphenethylamine and 4-phenylbutylamine (internal standard) were analyzed by gas chromatography-mass spectrum. The ions m/z 242 and m/z 91 were applied in quantitative analysis for 4-bromo-2, 5-dimethoxyphenethylamine and 4-phenylbutylamine, respectively. Results The limit of detection was 6 ng/mL in blood sample and the calibration curve was linear in the range of 0.02~10μg/mL (=0.9993) for 4-bromo-2, 5-dimethoxyphenethylamine. The RSDs of intra-day and inter-day were less than 10%; the average extraction recovery of 4-bromo-2, 5-dimethoxyphenethylamine was about 69%. Conclusions This method is rapid, sensitive and suitable for qualitative analysis of 4-bromo-2, 5-dimethoxyphenethylamine in blood.