A device for automated direct sampling and quantitation from solid-phase sorbent extraction cards by electrospray tandem mass spectrometry.
A device for automated direct sampling and quantitation from solid-phase sorbent extraction cards by electrospray tandem mass spectrometry.
复制标题
一种通过电喷雾串联质谱法从固相吸附剂萃取卡自动直接采样和定量的装置。
DOI：
10.1021/ac020501y
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发表时间：
2003
影响因子：
7.4
通讯作者：
J. Henion
中科院分区：
文献类型：
--
作者：
T. Wachs;J. Henion
一种新的固相萃取（SPE）装置，在96孔格式（SPE卡）已被用于自动离线样品制备的低容量尿样。在线自动分析物洗脱通过固相萃取和直接定量的微离子喷雾质谱报告。该样品制备装置具有微量滴定板的形式，并模制在塑料框架中，该塑料框架容纳96个单独的夹层3 M Empore吸附剂（0.5 mm厚，8微米颗粒），其两侧由微纤维支撑材料覆盖。96个离散的SPE区，每个直径为7 mm，以96孔微量滴定板的常规9 mm间距（间距）嵌入片中。在本研究中，SPE卡的四分之一（24个单独区域）仅用于方便。在从24个样品中对所施加的人尿液进行自动离线干扰洗脱后，将一段SPE卡垂直安装在配备有斜面尖端的微离子喷雾直接进样管前面的计算机控制的X，Y，Z定位器上。该针头的斜面尖端以连续方式自动穿透每个SPE洗脱区（吸附剂盘）或固定相。将洗脱的分析物顺序地直接转移到微电喷雾器中以获得串联质谱（MS/MS）分析。该策略排除了任何HPLC分离和相关方法开发。证明了从强化人尿样中定量测定利他林（哌甲酯）。哌甲酯的三氘代内标用于获得母体药物和内标之间的离子电流响应比。从6.6 ng/mL加标至3300 ng/mL的人对照尿样（在其他研究中已确定正常治疗水平为50 - 100 ng/mL尿液），并获得线性校准曲线，相关系数为0.9999，其中质控（QC）样品的精密度范围为24 ng/mL QC水平下的9.6%至3000 ng/mL QC水平下的1.2%，四个水平质控品的准确度范围为98.1%~ 100.3%。制备4种浓度的QC样品，分别为24、240、1200和3000 ng/mL。本工作中每个样品的运行时间为1.5 min，不包括样品制备时间。
A new solid-phase extraction (SPE) device in the 96-well format (SPE Card) has been employed for automated off-line sample preparation of low-volume urine samples. On-line automated analyte elution via SPE and direct quantitation by micro ion spray mass spectrometry is reported. This sample preparation device has the format of a microtiter plate and is molded in a plastic frame which houses 96 separate sandwiched 3M Empore sorbents (0.5-mm-thickness, 8-microm particles) covered on both sides by a microfiber support material. Ninety-six discrete SPE zones, each 7 mm in diameter, are imbedded into the sheet in the conventional 9-mm pitch (spacing) of a 96-well microtiter plate. In this study one-quarter of an SPE Card (24 individual zones) was used merely as a convenience. After automated off-line interference elution of applied human urine from 24 samples, a section of SPE Card is mounted vertically on a computer-controlled X, Y, Z positioner in front of a micro ion spray direct sampling tube equipped with a beveled tip. The beveled tip of this needle robotically penetrates each SPE elution zone (sorbent disk) or stationary phase in a serial fashion. The eluted analytes are sequentially transferred directly to a microelectrosprayer to obtain tandem mass spectrometric (MS/MS) analysis. This strategy precludes any HPLC separation and the associated method development. The quantitative determination of Ritalin (methylphenidate) from fortified human urine samples is demonstrated. A trideuterated internal standard of methylphenidate was used to obtain ion current response ratios between the parent drug and the internal standard. Human control urine samples fortified from 6.6 to 3300 ng/mL (normal therapeutic levels have been determined in other studies to be between 50 and 100 ng/mL urine) were analyzed and a linear calibration curve was obtained with a correlation coefficient of 0.9999, where the precision of the quality control (QC) samples ranged from 9.6% at the 24 ng/mL QC level to 1.2% at the 3000 ng/mL QC level, and the accuracy for the four levels of QC samples ranged from 98.1% to 100.3%. The QC samples were prepared at four concentrations which included 24, 240, 1200, and 3000 ng/mL, respectively. The run time per sample in this work was 1.5 min not including the sample preparation time.