Department of Environmental Science and Engineering, Fudan University, Shanghai 200433, China.
Anal Chem. 2010 Nov 15;82(22):9188-93. doi: 10.1021/ac102356r. Epub 2010 Oct 15.
Current direct analysis methods in mass spectrometry (MS) are predominantly focused on desorbing and ionizing samples in the solid phase. Some sampling difficulties are associated with liquid (solution) or gas samples. The present study has expanded direct MS analysis to solution samples by using the desorption corona beam ionization (DCBI) technique in combination with poly(dimethylsiloxane) (PDMS) substrate sampling. Typically, the PDMS substrate is dipped in water for microextraction of pesticide compounds and then is transferred to an MS ion source for desorption and ionization. This approach improves the detection limit for DCBI and allows more organic compounds in complex mixtures to be identified within seconds. The practical application of this device is demonstrated by identifying five pesticides (acephate, isoprocarb, dimethoate, dichlorvos, and dicofol) in water. The obtained detection limits of pesticides are 1 μg/L, the measured dynamic ranges are 3 orders of magnitude, the calculated correlation coefficients are between 0.939 and 0.979 at concentration levels of 5-5000 μg/L, and the repeatabilities defined as a relative standard deviation of five successive injections are in the range of 13-17%. The results indicate that the DCBI technique coupled with PDMS sampling is an excellent method for the analysis of organic pesticides in solution, and it also opens up a new avenue for direct MS studies of solution samples with general importance.
目前,质谱(MS)中的直接分析方法主要集中在固相中的样品解吸和离子化。一些与液体(溶液)或气体样品相关的采样困难。本研究通过使用解吸电晕束电离(DCBI)技术与聚二甲基硅氧烷(PDMS)基质采样相结合,将直接 MS 分析扩展到溶液样品。通常,将 PDMS 基质浸入水中进行农药化合物的微萃取,然后将其转移到 MS 离子源进行解吸和离子化。这种方法提高了 DCBI 的检测限,并允许在几秒钟内识别复杂混合物中的更多有机化合物。通过在水中鉴定五种农药(乙酰甲胺磷、异丙威、乐果、敌敌畏和三氯杀螨醇)来证明该设备的实际应用。获得的农药检测限为 1μg/L,测量的动态范围为 3 个数量级,在 5-5000μg/L 的浓度水平下计算的相关系数在 0.939 到 0.979 之间,五次连续进样的重复性定义为相对标准偏差在 13-17%范围内。结果表明,DCBI 技术与 PDMS 采样相结合是分析溶液中有机农药的一种极好方法,它也为直接 MS 研究具有普遍重要性的溶液样品开辟了新途径。