Karimi Akarm, Alizadeh Naader
Department of Chemistry, Faculty of Science, Bu-Ali Sina University, Hamadan, Iran.
Talanta. 2009 Jul 15;79(2):479-85. doi: 10.1016/j.talanta.2009.04.016. Epub 2009 Apr 16.
A rapid, simple, and sensitive headspace solid phase microextraction coupled to ion mobility spectrometry (HS-SPME-IMS) method is presented for analysis of the highly specific angiotensin-converting enzyme (ACE) inhibitor, captopril (CAP). Positive ion mobility spectra of CAP were acquired with an ion mobility spectrometer equipped with a corona discharge ionization source. Mass-to-mobility correlation equation was used to identify product ions. A dodecylsulfate-doped polypyrrole (PPy-DS) coating was used as a fiber for SPME. The results showed that PPy-DS based SPME fiber was suitable for successfully extracting CAP from human blood plasma and pharmaceutical samples. The HS-SPME-IMS method provided good repeatability (R.S.D.s<4%) for aqueous and spiked plasma samples. The calibration graphs were linear in the range of 10-300 ng mL(-1) (R(2)>0.99) and detection limits were 7.5 ng mL(-1) for aqueous and 6.3 ng mL(-1) for plasma blank samples. Finally, a standard addition calibration method was applied to HS-SPME-IMS technique for the analysis of blood plasma samples and tablets. Purpose method seemed to be suitable for the analysis of CAP in plasma samples as it is not time consuming (state total time from sample preparation to analysis), it required only small quantities of the sample, and no derivatization was required.
本文提出了一种快速、简单且灵敏的顶空固相微萃取-离子迁移谱联用（HS-SPME-IMS）方法，用于分析高特异性血管紧张素转换酶（ACE）抑制剂卡托普利（CAP）。使用配备电晕放电电离源的离子迁移谱仪采集了CAP的正离子迁移谱。采用质荷比-迁移率相关方程来识别产物离子。以十二烷基硫酸盐掺杂的聚吡咯（PPy-DS）涂层作为固相微萃取的纤维。结果表明，基于PPy-DS的固相微萃取纤维适用于从人血浆和药物样品中成功萃取CAP。HS-SPME-IMS方法对水性样品和加标血浆样品具有良好的重复性（相对标准偏差<4%）。校准曲线在10 - 300 ng mL⁻¹范围内呈线性（R²>0.99），水性样品的检测限为7.5 ng mL⁻¹，血浆空白样品的检测限为6.3 ng mL⁻¹。最后，将标准加入校准法应用于HS-SPME-IMS技术，用于分析血浆样品和片剂。目标方法似乎适用于血浆样品中CAP的分析，因为它不耗时（从样品制备到分析的总时间），仅需少量样品，且无需衍生化。
