Rapid Determination of Organophosphorus Pesticides on Surfaces of Fruits and Vegetables by MS/MS with Desorption Electrospray Ionization
摘 要
在不需要样品制备、预处理的前提下,将电喷雾解吸串联质谱法用于果蔬表面残留的乙酰甲胺磷、甲拌磷、乐果、乙嘧硫磷、乙硫磷和亚胺硫磷等6种有机磷农药的直接快速检测。在串联质谱中,选择电喷雾离子源,用甲醇作雾化溶剂;以碰撞诱导解离反应正离子检测模式进行定性和定量检测。确定了上述6种有机磷农药的碎片特征峰(m/z)分别为206,261,252,293,407,318。结果表明:6种有机磷农药分子的裂解规律与其分子结构相吻合,排除了检测结果的假阳性。方法的检出限(3S/N)在5.0×10-10~1.0×10-8g·cm-2之间。以1.0×10-8g·cm-2的6种有机磷农药溶液进样,平行测定8次,测定值的相对标准偏差在1.6%~6.5%之间。
Abstract
Desorption electrospray ionization-tandem mass spectrometry (DESI-MS/MS) was applied to the rapid determination of residual amounts of 6 organophosphorus pesticides (OPP′s), i.e., acephate, thimet, rogor, etrimfos, ethion and phosemet, on surface of fruits and vegetables, without sample preparation and pretreatment. In the MS/MS analysis, ESI was used as ion ization source with methanol as the electrospray solvent, and positive electrospray ionization as well as collision induced dissociation reaction monitoring mode was taken for qualitative and quantitative analysis. The characteristic peaks of the fragments of 6 organophosphorous pesticides with (m/z) 206, 261, 230, 293, 407, 340 respectively were confirmed. It was found that the fragmentation regularity of molecules of the 6 OPP′s were in coincidence with their molecular structures, and the possibility of arising false positiveness of the results of detection was thus eliminated. Values of detection limit (3S/N) found were in the range of 5.0×10-10-1.0×10-8g·cm-2. Precision of the method was tested with sample introduction of 1.0×10-8g·cm-2 of mixture of the 6 OPP′s for 8 determinations, values of RSD′s found were in the range of 1.6%-6.5%.
中图分类号 O657.63
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基金项目 2010福建省教育厅B类项目(JB10191)
收稿日期 2011/5/9
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备注薛岚(1967-),男,福建宁德人,副教授,主要研究方向为分析化学与环境化学。
引用该论文: XUE Lan,SU Hai-feng. Rapid Determination of Organophosphorus Pesticides on Surfaces of Fruits and Vegetables by MS/MS with Desorption Electrospray Ionization[J]. Physical Testing and Chemical Analysis part B:Chemical Analysis, 2011, 47(10): 1218~1221
薛岚,苏海峰. 电喷雾解吸电离串联质谱法快速检测果蔬表面残留有机磷农药[J]. 理化检验-化学分册, 2011, 47(10): 1218~1221
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参考文献
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【2】BLASCO C,FONT G,PICO Y. Analysis of pesticides in fruits by pressurized liquid extraction and liquid chromatography-ion trap-triple stage mass spectrometry[J]. J Chromatogr A, 2005,1098(1/2):37-37.
【3】GOTO T, ITO Y, YAMADA S, et al. The high throughput analysis of N-methyl carbamate pesticides in fruits and vegetables by liquid chromatography electrospray ionization tandem mass spectrometry using a short column[J]. Anal Chim Acta, 2006,555(2):225-226.
【4】NOGUERIA J, SANDRA T, SANDRA P. Multiresidue screening of neutral pesticides in water samples by high performance liquid chromatography-electrospray mass spectrometry[J]. Anal Chim Acta, 2004,505(2):209-210.
【5】KOCHMAN M, GORDIN A, GOLDSHLAG P, et al. Fast, high-sensitivity, Multipesticide analysis of complex mixtures with supersonic gas chromatography-mass spectrometry[J]. J Chromatogr A, 2002,974(1/2):185-186.
【6】邹明强,杨蕊,赵丽丽,等.用手持式农药速测仪酶法现场测定蔬菜中有机磷及氨基甲酸酯农药残毒[J].高等学校化学学报, 2003,24(6):1016-1017.
【7】黄永春,刘红梅,裴瑞瑞,等.应用固化酶检测黄瓜中氨基甲酸酯类农药[J].环境科学, 2006,27(7):1469-1469.
【8】TAKATS Z, WISEMAN J M, COOKS R G, et al. Mass spectrometry sampling under ambient conditions with desorption electrospray ionization[J]. Science, 2004,306(5695):471-472.
【9】TAKATS Z, COTTE R, COOKS R G, et al. Direct, trace level detection of explosives on ambient surfaces by desorption electrospray ionization mass spectrometry[J]. Chem Commun, 2005(15):1950-1951.
【10】WILLIAMS J, LOCK R, PATEL V, et al. Polarity switching accurate mass measurement of pharmaceutical samples using desorption electrospray ionization and a dual ion source interfaced to an orthogonal acceleration time-of-flight mass spectrometer[J]. Anal Chem, 2006,78(21):7440-7441.
【11】陈焕文,李明,周建光,等.电喷雾解析电离质谱法用于临床尿样的直接分析[J].高等学校化学学报, 2006,27(8):1439-1440.
【12】陈焕文,张燮,罗明标.电喷雾解析电离质谱法对食品中苏丹红染料的快速检测[J].分析化学, 2006,34(4):464-465.
【13】陈焕文,赖劲虎,周瑜芬,等.表面解吸常压化学电离源的研制及应用[J].分析化学, 2007,35(8):1233-1234.
【14】梁华正,陈焕文.表面解吸常压化学电离质谱法快速测定茶叶化学指纹图谱[J].应用化学, 2008,25(5):519-520.
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