Barroso M, Gallardo E, Margalho C, Avila S, Marques E P, Vieira D N, López-Rivadulla M
Instituto Nacional de Medicina Legal, Delegação de Coimbra, Largo da Sé Nova, 3000-213 Coimbra, Portugal.
J Chromatogr B Analyt Technol Biomed Life Sci. 2005 Feb 25;816(1-2):29-34. doi: 10.1016/j.jchromb.2004.10.071.
A simple and rapid method based on solid phase microextraction (SPME) via direct immersion followed by gas chromatography coupled with electron impact ionization/mass spectrometry (GC/EI-MS) was developed for the determination of strychnine in blood. Papaverine was used as internal standard (I.S.). Two types of fibre coating were tested, 100 microm polydimethylsiloxane and 65 microm Carbowax/Divinylbenzene, the latter giving higher recoveries of the compound. The main factors affecting the SPME process, such as sample dilution (1:10), adsorption and desorption times (20 and 10 min, respectively), carry-over effect (not observed), pH and salt addition (no modifications on pH or salt concentration) were optimized. The procedure was validated in terms of linearity (r(2)=0.9992 for concentrations ranging from 0.10 to 5.00 microg/mL), intra and interday precision (0.93 and 4.62%, respectively at 0.50 microg/mL; 3.33 and 8.06%, respectively at 2.50 microg/mL), sensitivity (6.83 and 8.91 ng/mL for LOD and LOQ, respectively) and extraction recovery (0.54 and 0.39% at 0.50 and 2.50 microg/mL, respectively). The developed procedure was found suitable for forensic investigations and was considered a good alternative to the liquid-liquid extraction methods normally used for the determination of this compound in biological media.
建立了一种基于直接浸入式固相微萃取(SPME),随后进行气相色谱-电子轰击电离/质谱联用(GC/EI-MS)的简单快速方法,用于测定血液中的士的宁。以罂粟碱作为内标物(I.S.)。测试了两种类型的纤维涂层,100μm聚二甲基硅氧烷和65μm聚乙二醇/二乙烯基苯,结果表明后者对该化合物的回收率更高。对影响SPME过程的主要因素进行了优化,如样品稀释度(1:10)、吸附和解吸时间(分别为20分钟和10分钟)、残留效应(未观察到)、pH值和盐添加量(pH值或盐浓度未作调整)。该方法在以下方面得到了验证:线性(浓度范围为0.10至5.00μg/mL时,r(2)=0.9992)、日内和日间精密度(在0.50μg/mL时分别为0.93%和4.62%;在2.50μg/mL时分别为3.33%和8.06%)、灵敏度(检测限和定量限分别为6.83和8.91 ng/mL)以及萃取回收率(在0.50和2.50μg/mL时分别为0.54%和0.39%)。结果表明,所建立的方法适用于法医调查,是生物介质中该化合物测定通常采用的液-液萃取方法的良好替代方法。