| 超高效液相色谱－串联质谱法同时测定血液和尿液中10种2C系列苯乙胺类衍生物 |
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| 基金项目:中央级公益性科研院所基本科研业务费项目（2021JB007）；中央高校基本科研业务费项目（2022JKF02005） |
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| 中文摘要:该文建立了同时检测血液、尿液样本中2C－H、2C－D、2C－P、2C－T－2、2C－T－4、2C－T－7、25D－NBOMe、25C－NBOMe、25B－NBOMe和25I－NBOMe 10种2C系列苯乙胺类衍生物含量的超高效液相色谱－串联质谱（UPLC－MS/MS）法。通过比较沉淀蛋白（PPT）、液－液萃取（LLE）和固相萃取（SPE）3种前处理方法，选用甲醇沉淀蛋白法对血液和尿液样品进行提取。通过对色谱柱和流动相的优化，选用甲醇－水（0.1%甲酸）作为流动相，ACQUITY UPLC?BEH C18（100 mm × 2.1 mm，1.7 μm）色谱柱进行分离。串联质谱的离子源为电喷雾电离源（ESI+），采用多反应监测模式（MRM）进行检测。10种目标物在0.005 ~ 50 ng/mL范围内线性关系良好，相关系数（r2）为0.995 8 ~ 0.999 9。血液和尿液中的检出限分别为0.01 ~ 2 ng/mL和0.002 ~ 5 ng/mL，3个不同加标浓度（1、5、20 ng/mL）下，血液、尿液中的基质效应为71.9%~112%，提取回收率为78.8% ~ 99.3%，日内、日间相对标准偏差（RSD，n = 3）均不高于15%。该方法分离效果好，提取回收率高，基质效应低，且操作简便，检材用量少，适用于血液和尿液中2C系列苯乙胺类衍生物的快速检测。 |
| 中文关键词:超高效液相色谱－串联质谱法 血液 尿液 2C系列苯乙胺类衍生物 |
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| Simultaneous Determination of 10 2C-series Phenethylamines in Blood and Urine by UPLC－MS/MS |
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| Abstract:An ultra-high performance liquid chromatography－tandem mass spectrometry（UPLC－MS/MS） was established for the simultaneous detection of 10 2C-series phenethylamines，i.e．2C－H，2C－D，2C－P，2C－T－2，2C－T－4，2C－T－7，25D－NBOMe，25C－NBOMe，25B－NBOMe and 25I－NBOMe in blood and urine samples．Comparing three preparation methods respectively，including precipitated protein（PPT），liquid－liquid extraction（LLE） and solid phase extraction（SPE），blood and urine samples were finally extracted by precipitated protein method with methanol．The chromatographic column and mobile phase were also optimized in this experiment．ACQUITY UPLC? BEH C18（100 mm × 2.1 mm，1.7 μm） was finally used as the analytical column to separate the targeted analytes with methanol－water（0.1% formic acid） solution as the mobile phase．The ion source of the tandem mass spectrometer was electrospray ionization（ESI），which was performed in multiple reaction monitoring（MRM） mode．There were good linear relationships for 10 target compounds in the range of 0.005－50 ng/mL，with the correlation coefficients（r2） of 0.995 8－0.999 9．The limits of detection（LODs） for 10 2C-series phenethylamines in blood and urine were in the range of 0.01－2 ng/mL and 0.002－5 ng/mL，respectively．At three spiked concentration levels of 1，5 and 20 ng/mL，the matrix effects for 10 target compounds in blood and urine were in the range of 71.9%－112%，and the recoveries ranged from 78.8% to 99.3%，with the intra-day and inter-day relative standard deviations（RSDs） both not more than 15%．This method is characterized by rapid analysis，simple operation，high detection sensitivity，small sampling amount，accurate results and good repeatability，and is suitable for the rapid determination of 2C-series phenethylamines in blood and urine. |
| Key Words:ultra-high performance liquid chromatography－tandem mass spectrometry blood urine 2C-series phenethylamines |
| 引用本文：李锦昌，何洪源，张云峰，王瑞花.超高效液相色谱－串联质谱法同时测定血液和尿液中10种2C系列苯乙胺类衍生物[J].分析测试学报,2022,41(11):1614-1620. |
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