固相微萃取-气相色谱-质谱法测定大头金蝇样本内氯氮平  

Determination of Clozapine Concentration in Samples of Chrysomya Megacephala by Solid-Phase Microextraction(SPME)-GC/MS

作　　者：李学博[1] 莫耀南[2] 周海梅[2] 李朴[2] 马锦琦[2] 万立华[1] 王清山[3] 

机构地区：[1]重庆医科大学法医学与生物医学信息研究室,重庆400016 [2]河南科技大学法医学院,河南洛阳471003 [3]重庆市公安局物证鉴定中心,重庆401147

出　　处：《质谱学报》2012年第3期186-191,共6页Journal of Chinese Mass Spectrometry Society

摘　　要：为了探索嗜尸性蝇类样本内氯氮平的有效检测方法及可靠性,为氯氮平中毒死亡案件的法医学检验分析提供新途径,采用固相微萃取结合气相色谱-质谱联用(SPME-GC/MS)的方法,对大头金蝇幼虫及蛹样本内的氯氮平进行定量分析检测。以100μm聚二甲基硅氧烷萃取头萃取,洛沙平为内标,气相色谱-质谱选择离子方式,检测不同发育时期,取食含有不同浓度水平氯氮平的肌肉组织的大头金蝇样本。结果表明,氯氮平检出限为0.1μg/L,在5～5000μg/L范围内线性良好,不同浓度的回收率在93%～104%间,日内及日间精密度(RSD)均小于8%。该方法简便快捷,精密度好,结果可靠,能准确定量检测昆虫样本内的氯氮平,可用于此类中毒案件中的法医学分析。To explore effective detection methods and so as to offer a new detection methods and forensic medical analysis strategies for this kind of poisoning cases a method of solidphase microextraction （SPME）-gas chromatography-mass spectrometry （GC/MS） was established to determine clozapine concentration in samples of Chrysomya megacephala fed on different diet substrate added a certain amount of clozapine at different developmental stages including larvae and pupae. The clozapine was extracted by 100μm polydimethylsiloxane （PDMS） fiber. Loxapine was used as internal standard and detected by GC/MS in selected ion monitoring （SIM）. The analytical results showed that the detection limit of clozapine was 0.1μg/L. The standard curve was linear in the range of 5-5 000 μg/L. The average recovery of clozapine in the range of 93 %-104% in different concentration. The precisions （RSD） of inter-day and intra-day was less than 8%. This method was validated with respect to simplicity, accuracy and precision and provided a new potential effective detection strategies. It can he used for analysis of necrophagous flies samples in this kind of toxic poisoning cases.

关 键 词：固相微萃取(SPME) 气相色谱-质谱法(GC/MS) 氯氮平 昆虫样本 

分 类 号：O657.63[理学—分析化学]