Shahar T, Dagan S, Amirav A
School of Chemistry, Sackler Faculty of Exact Sciences, Tel Aviv University, Israel.
J Am Soc Mass Spectrom. 1998 Jun;9(6):628-37. doi: 10.1016/S1044-0305(98)00016-6.
A novel method for fast analysis is presented. It is based on laser desorption injection followed by fast gas chromatography-mass spectrometry (GC-MS) in supersonic molecular beams. The sample was placed in an open air or purged laser desorption compartment, held at atmospheric pressure and near room temperature conditions. Desorption was performed with a XeCl Excimer pulsed laser with pulse energy of typically 3 mJ on the surface. About 20 pulses at 50 Hz were applied for sample injection, resulting in about 0.4 s injection time and one or a few micrograms sample vapor or small particles. The laser desorbed sample was further thermally vaporized at a heated frit glass filter located at the fast GC inlet. Ultrafast GC separation and quantification was achieved with a 50-cm-long megabore column operated with a high carrier gas flow rate of up to 240 mL/min. The high carrier gas flow rate provided effective and efficient entrainment of the laser desorbed species in the sweeping gas. Following the fast GC separation, the sample was analyzed by mass spectrometry in supersonic molecular beams. Both electron ionization and hyperthermal surface ionization were employed for enhanced selectivity and sensitivity. Typical laser desorption analysis time was under 10 s. The laser desorption fast GC-MS was studied and demonstrated with the following sample/matrices combinations, all without sample preparation or extraction: (a) traces of dioctylphthalate plasticizer oil on stainless steel surface and the efficiency of its cleaning; (b) the detection of methylparathion and aldicarb pesticides on orange leaves; (c) water surface analysis for the presence of methylparathion pesticide; (d) caffeine analysis in regular and decaffeinated coffee powder; (e) paracetamol and codeine drug analysis in pain relieving drug tablets; (f) caffeine trace analysis in raw urine; (g) blood analysis for the presence of 1 ppm lidocaine drug. The features and advantages of the laser desorption fast GC-MS are demonstrated and discussed.
本文介绍了一种用于快速分析的新方法。该方法基于激光解吸进样,随后在超声分子束中进行快速气相色谱-质谱联用(GC-MS)分析。样品置于常压且接近室温条件下的开放式空气或吹扫激光解吸室中。使用脉冲能量通常为3 mJ的XeCl准分子脉冲激光在样品表面进行解吸。以50 Hz的频率施加约20个脉冲用于样品进样,进样时间约为0.4 s,可产生约一微克或几微克的样品蒸气或小颗粒。激光解吸的样品在快速气相色谱仪进样口处的加热烧结玻璃过滤器上进一步热蒸发。使用一根50 cm长的大口径柱,以高达240 mL/min的高载气流速实现了超快速气相色谱分离和定量分析。高载气流速有效地将激光解吸的物质夹带在吹扫气体中。快速气相色谱分离后,样品在超声分子束中进行质谱分析。同时采用电子电离和超热表面电离以提高选择性和灵敏度。典型的激光解吸分析时间在10 s以内。对激光解吸快速GC-MS进行了研究,并通过以下样品/基质组合进行了验证,所有这些均无需样品制备或萃取:(a)不锈钢表面痕量邻苯二甲酸二辛酯增塑剂油及其清洁效率;(b)橙叶上甲基对硫磷和涕灭威农药的检测;(c)水体表面甲基对硫磷农药的分析;(d)普通咖啡粉和脱咖啡因咖啡粉中的咖啡因分析;(e)止痛片中对乙酰氨基酚和可待因药物分析;(f)原尿中咖啡因痕量分析;(g)血液中1 ppm利多卡因药物的分析。展示并讨论了激光解吸快速GC-MS的特点和优势。