以分析有机磷农药为例研究多反应气-负化学电离源质谱的行为
Negative Chemical Ionization Mass Spectrometric Analysis with Different Reaction Gases for Determination of Organophosphorus Pesticides
-
摘要: 在气相色谱-质谱分析中,负化学电离源质谱特别适合于高电负性目标物的分析,但不同反应气的对比研究工作至今未见报道。本研究采用甲烷、异丁烷、氨气、甲烷+氨气混合气、异丁烷+氨气混合气作为反应气,在负化学离子源内对电负性较高的有机磷农药进行电离实验,对反应气压力、离子源温度、灯丝发射电流等多项参数进行了考察。结果表明:采用纯氨气作为反应气,检测背景低,质谱真空负荷小,并可在负化学源质谱上获得最高的灵敏度。配合加速溶剂萃取方法,对土壤中的有机磷农药残留进行分析,方法全流程回收率为73.3%~108.1%,精密度为2.5%~8.8%,检出限为0.01~0.32 μg/kg,各项指标均可满足实际样品测试需求。Abstract: Negative Chemical Ionization Mass Spectrometry (NCI-MS) is amenable to organic compounds with high electronegativity. However, nothing has previously been reported about the comparative study of a different reaction gas. In this paper, the methane, isobutane, ammonia, ammonia in methane, ammonia in isobutane as reaction gases for NCI are introduced. The effect factors of reaction gas pressure, source temperature, filament emission current and electron energy are evaluated for each high electronegativity pesticide considered in this study. Finally, the pure ammonia led to a remarkable reduction in background noise with a significant improvement for overall sensitivity of the method. Combining with ASE extraction, the limit of detection (LOD) for residue pesticides in soil is between 0.01-0.32 μg/kg, the recovery is 73.3%-108.1% and the RSD is between 2.5%~8.8%.
-
-
张莉,张永涛,桂建业.水中氯代酸性除草剂衍生气相色谱法主要要素分析探讨[J].中国环境监测,2011,27(4): 45-49. 董静,潘玉香,秦亚萍,余琼卫,骆丹.气相色谱-负化学离子源质谱法同时检测蔬菜中103种农药残留[J].分析科学学报,2010,26(3): 323-328. 刘磊,郭永泽,张玉婷,邵辉,李辉,宋淑荣.中药材中有机氯类农药的GC-NCI-MS分析[J].天津农业科学,2009,15(5): 34-36. 董静,潘玉香,秦亚萍,吕建霞,余琼卫.程序升温大体积进样气相色谱-负化学离子源质谱法测定白菜和苹果中103种农药残留[J].色谱,2010,28(7): 654-663. 王旭亮,何欢,李文超,杨绍贵,孙成.加速溶剂萃取/凝胶渗透色谱净化/气相色谱-负化学离子源质谱测定生物样品中的四溴联苯醚[J].环境化学,2011,30(6): 1186-1191. 沈伟健,林宏,赵增运,丁涛,徐锦忠,沈崇钰.固相分散萃取与气相色谱-负化学离子源质谱联用法测定食品中三唑醇的残留量[J].色谱,2008,26(4): 515-518. Renata B. Large volume cold on-column injection for gas chromatography-negative chemical ionization-mass spe-ctrometry analysis of selected pesticides in air samples[J]. Journal of Agricultural Food Chemistry, 2007, 55(4): 1150-1155. Renata B. Large volume cold on-column injection for gas chromatography-negative chemical ionization-mass spe-ctrometry analysis of selected pesticides in air samples[J]. Journal of Agricultural Food Chemistry, 2007, 55(4): 1150-1155.
Silvia L, Míriam G. Validation of a pressurized solvent extraction and GC-NCI-MS method for the low level determination of 40 polybrominated diphenyl ethers in mothers' milk[J].Chemosphere,2008,73(1): 70-75. Silvia L, Míriam G. Validation of a pressurized solvent extraction and GC-NCI-MS method for the low level determination of 40 polybrominated diphenyl ethers in mothers' milk[J].Chemosphere,2008,73(1): 70-75.
Patrick R, Burnaby M. Effect of ammonia partial pressure on the sensitivities for oxygenated compounds in ammonia chemical ionization mass spectrometry[J]. Analytical Chemistry, 1986, 58(14): 2903-2907. Patrick R, Burnaby M. Effect of ammonia partial pressure on the sensitivities for oxygenated compounds in ammonia chemical ionization mass spectrometry[J]. Analytical Chemistry, 1986, 58(14): 2903-2907.
Murty M R V S, Prabhakar S, Lakshmi V V S, Vijaya S U V R, Jagadeshwar R T, Vairamani M. Mass spectral analysis of chloropicrin under negative ion chemical ionization conditions [J].Analytical Chemistry, 2005,77(10): 3406-3410. Murty M R V S, Prabhakar S, Lakshmi V V S, Vijaya S U V R, Jagadeshwar R T, Vairamani M. Mass spectral analysis of chloropicrin under negative ion chemical ionization conditions [J].Analytical Chemistry, 2005,77(10): 3406-3410.
Renata R, Patricia H. Comparison of gas chromatography-mass spectrometry and gas chromatography-tandem mass spectrometry with electron ionization and negative-ion chemical ionization for analyses of pesticides at trace levels in atmospheric samples [J]. Analytical Chemistry Insights, 2008, 3: 111-125. Renata R, Patricia H. Comparison of gas chromatography-mass spectrometry and gas chromatography-tandem mass spectrometry with electron ionization and negative-ion chemical ionization for analyses of pesticides at trace levels in atmospheric samples [J]. Analytical Chemistry Insights, 2008, 3: 111-125.
桂建业,张莉,齐继祥,张永涛,左海英,张琳,李桂香.固相萃取衍生气相色谱-负化学源质谱法检测水中酸性除草剂[J].分析化学,2010,38(8): 1177-1181. Lacorte S, Barcelo D. Rapid degradation offenitrothion in estuarine waters[J]. Environmental Science and Technology, 1994, 28(6): 1159-1163. Lacorte S, Barcelo D. Rapid degradation offenitrothion in estuarine waters[J]. Environmental Science and Technology, 1994, 28(6): 1159-1163.
Munch D J, Frebis C P. Analyte stability studies con-ducted during the national pesticide survey[J]. Environmental Science and Technology,1992, 26(5): 921-925. Munch D J, Frebis C P. Analyte stability studies con-ducted during the national pesticide survey[J]. Environmental Science and Technology,1992, 26(5): 921-925.
李宏亮,蒋志华,汪志新.饮用水中六种有机磷农药国标测定方法的改进[J].中国卫生检验杂志,2010,20(12): 3498-3499. 王一龙,杨敏, 董春洲.顶空固相微萃取-气相色谱法分析水中5 种有机磷农药[J].华中师范大学学报: 自然科学版,2006,40(3): 375-378. 杨元,高玲,景露.SPE-GC/MS法测定水中有机磷农药和氨基酸酯农药[J].中国测试,2009,35(2): 86-89. 许鹏翔,袁东星,邓永智.水样中痕量有机磷农药的膜萃取-气相色谱法测定[J].分析化学,2002,30(3): 321-323. 李朴,周海梅,马锦崎.水中微量甲胺磷农药的检验[J].河南科技大学学报: 医学版,2006,24(1): 59-60. St-Amand A D, Louise G. Determination of acephate and its degradation product methamidophos in soil and water by solid-phase extraction (SPE) and GC-MS[J]. Environmental Analytical Chemistry, 2004, 84(10): 739-748. St-Amand A D, Louise G. Determination of acephate and its degradation product methamidophos in soil and water by solid-phase extraction (SPE) and GC-MS[J]. Environmental Analytical Chemistry, 2004, 84(10): 739-748.
贺敏,陶传江,姜辉.乙酰甲胺磷在水中消解和残留动态研究[J].农药科学与管理,2007,25(2): 13-16. 宋淑玲,李重九,马晓东.蔬菜中残留农药的石墨化碳黑净化和气相色谱-质谱检测方法[J].分析化学,2008,36(11): 1526-1530. US EPA Method 3545A, Pressurized Fluid Extraction (PFE) [S]. 2000. US EPA Method 3545A, Pressurized Fluid Extraction (PFE) [S]. 2000.
陈耀祖,涂亚平.有机质谱原理及应用[M].北京: 科学出版社,2004: 70. Adams N G, Babcock L M. Advances in Gas Phase Ion Chemistry [M].Greenwich: JAI Press, 1998. Adams N G, Babcock L M. Advances in Gas Phase Ion Chemistry [M].Greenwich: JAI Press, 1998.
计量
- 文章访问数: 1650
- HTML全文浏览量: 0
- PDF下载量: 1471
下载:
京公网安备 11010202008159号