建立了水果和蔬菜中三环锡、三苯锡和苯丁锡同时检测的格氏试剂衍生-气相色谱-串联质谱方法（ GC-MS /MS）。样品经盐酸/四氢呋喃（1：10，v / v）消解，正己烷振荡提取，乙基溴化镁衍生和 Florisil 固相萃取净化，采用GC-MS / MS 多反应监测（MRM）模式对3种有机锡化合物进行定性和定量分析。实验结果表明，以苹果为代表性样品基质，三环锡、三苯锡和苯丁锡的检出限（ LOD）分别为2.0、1.5和3.4μg / kg（以 Sn 计），在10、20、50、200μg / kg（以 Sn 计）共4个添加水平下的平均回收率为72.4％~107.1％，相对标准偏差为0.4％~14.2％。该方法灵敏度高，选择性强，可以实现3种有机锡农药的同时检测，能够满足国内外残留限量的检测要求。
A method for the simultaneous determination of cyhexatin,triphenyltin and fenbuta-tin oxide residues in fruits and vegetables was developed by Grignard derivatization and gas chromatography coupled to tandem mass spectrometry(GC-MS / MS). The samples were firstly digested by HCl / THF(1 :10,v / v),then extracted by hexane and followed by the derivatization with Grignard reagent(EtMgBr). Then after purification using florisil SPE columns,the sample extracts were finally analyzed by GC-MS / MS. The qualitative and quantitative determinations of the three organotin pesticides were performed by the tandem mass in multiple reaction monito-ring(MRM)mode. By using apple as a representative matrix,the limits of detection( LODs) obtained by the proposed method for cyhexatin,triphenyltin and fenbutatin oxide were 2. 0,1. 5 and 3. 4 μg / kg(as Sn),respectively. The average recoveries for the three organotin pesticides were in the range of 72. 4% -107. 1% at the spiked levels of 10,20,50 and 200 μg / kg( as Sn) and the relative standard deviations(RSDs)ranged from 0. 4% to 14. 2% . The proposed method was validated to have good linearity,high sensitivity,selectivity and accuracy for the simulta-neous determination of cyhexatin,triphenyltin and fenbutatin oxide in fruits and vegetables. The sensitivity of this method can meet the requirements of the inspection for the three organotin pesticides at the level of maximum residue limits(MRLs)set by China and some other countries.
参考文献
| [1] | Jiang Q,Shi P F,Hu X L. Chemical Reagents(姜琴,施鹏飞,胡喜兰. 化学试剂),2011,33(11):1014,2011. |
| [2] | Campillo N,Vinas P,Penalver R,et al. J Food Compos Anal,2012,25(1):66,2012. |
| [3] | Li D L. Physical Testing and Chemical Analysis Part B:Chemical Analysis(李德良. 理化检验:化学分册),2010,46 (5):518,2010. |
| [4] | GB/T 5009. 215-2008,2008. |
| [5] | Montes R,Canosa P,Lamas J P,et al. Anal Bioanal Chem, 2009,395(8):2601,2009. |
| [6] | Canosa P,Montes R,Lamas J P,et al. Talanta,2009,79 (3):598,2009. |
| [7] | Wu M,Lu J,Zhu Y H,et al. Chinese Journal of Pesticide Science(吴珉,卢军,朱亚红,等. 农药学学报),2011,13 (5):503,2011. |
| [8] | SN 0592-1996,1996. |
| [9] | Devos C,Moens L,Sandra P. J Sep Sci,2005,28(7):665,2005. |
| [10] | Wang J H,Zhao L,Cai F,et al. Food Science(王建华,赵亮,蔡发,等. 食品科学),2007,28(9):446,2007. |
| [11] | SN/T 1990-2007,1990. |
| [12] | SN/T 3149-2012,2012. |
| [13] | Zhu W X,Liu Y F,Yang J Z. Chinese Journal of Chroma-tography(祝伟霞,刘亚风,杨冀州. 色谱),2010,28(9):867,2010. |
| [14] | Vercauteren J,De Meester A,De Smaele T,et al. J Anal Atom Spectrom,2000,15(6):651,2000. |
| [15] | Gao W P,Hu X G,Sun S J,et al. Chinese Journal of Spec-troscopy Laboratory(高伟平,胡新功,孙书军,等. 光谱实验室),2006,23(6):1143,2006. |
| [16] | Jiang S X,Feng J J. Chinese Journal of Chromatography (蒋生祥,冯娟娟. 色谱),2012,30(3):219,2012. |
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