Quantitation of SR 27417 in human plasma using electrospray liquid chromatography tandem mass spectrometry: A study of ion suppression
Quantitation of SR 27417 in human plasma using electrospray liquid chromatography tandem mass spectrometry: A study of ion suppression
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DOI：
10.1016/s1044-0305(96)00072-4
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发表时间：
1996-11-01
影响因子：
3.2
通讯作者：
Rudewicz, PJ
中科院分区：
文献类型：
--
作者：
Buhrman, DL;Price, PI;Rudewicz, PJ
采用电喷雾液相色谱-串联质谱法检查了共洗脱基质化合物对人血浆中SR 27417定量的影响。在本试验的方法开发阶段，使用三种不同的程序提取加标100 pg/mL分析物的血浆样品：己烷液-液萃取、乙酸乙酯反萃取和固相萃取。分析物的离子强度被认为是成反比的共洗脱基质成分的电离百分比证明了全扫描光谱。乙酸乙酯反萃取，其中含有最少的共洗脱组分，导致在最高的离子强度的分析物。通过使用用于样品制备的液-液己烷和乙酸乙酯反萃取进行含量测定比较。重复1 mL，提取并分析5 - 2000 pg/mL 11个浓度的样品（n = 5）。乙酸乙酯反萃取样品的结果在2000 - 5 pg/mL范围内可接受，准确度范围为标称浓度的-11.6%至2.61%。相比之下，己烷液-液法在低于20 pg/mL时准确度和精密度较差。这种差异可以通过抑制分析物离子强度来解释。这些结果与目前的电喷雾电离理论是一致的。(C)1996年美国质谱学会
The effect of coeluting matrix compounds on the quantitation of SR 27417 in human plasma using electrospray liquid chromatography-tandem mass spectrometry has been examined. During the method development stage of this assay, plasma samples spiked with the analyte at 100 pg/mL were extracted using three different procedures: a hexane liquid-liquid extraction, an ethyl acetate back-extraction, and a solid phase extraction. Ion intensity of the analyte was found to be related inversely to the percent ionization of coeluting matrix components as evidenced by full scan spectra. The ethyl acetate back-extraction, which contained the fewest coeluting components, resulted in the highest ion intensity for the analyte. An assay comparison was done by using the liquid-liquid hexane and the ethyl acetate back-extractions for sample preparation. Replicate 1-mL, samples (n = 5) at 11 concentrations from 5 to 2000 pg/mL were extracted and analyzed. The results for the ethyl acetate back-extracted samples were acceptable from 2000 to 5 pg/mL with accuracy ranging from -11.6 to 2.61% of the nominal concentrations. In contrast, the hexane liquid-liquid method had poor accuracy and precision below 20 pg/mL. The difference is explained by suppression of analyte ion intensity. These results are consistent with the current theory of electrospray ionization. (C) 1996 American Society for Mass Spectrometry