Citation: CAO Zhaoyun, MOU Renxiang, WU Li, LIN Xiaoyan, ZHU Zhiwei, CHEN Mingxue. Combination of programmable temperature vaporizer-large volume injection gas chromatography-mass spectrometry and automated mass spectral deconvolution and identification system for the determination of 32 pesticides in fruits and vegetables[J]. Chinese Journal of Chromatography, ;2014, 32(12): 1390-1399. doi: 10.3724/SP.J.1123.2014.09005 shu

Combination of programmable temperature vaporizer-large volume injection gas chromatography-mass spectrometry and automated mass spectral deconvolution and identification system for the determination of 32 pesticides in fruits and vegetables

CAO Zhaoyun ^1,2 ,
MOU Renxiang ^1,2 ,
WU Li ^1,2 ,
LIN Xiaoyan ^1,2 ,
ZHU Zhiwei ^1,2 ,
CHEN Mingxue ^1,2,,

1.
1. Rice Product Quality Inspection and Supervision Center, Ministry of Agriculture, China National Rice Research Institute, Hangzhou 310006, China;

Corresponding author: CHEN Mingxue,
Received Date: 3 September 2014
Available Online: 13 October 2014
Fund Project: 国家粮油作物产品质量安全风险评估项目(GJFP2014006). (GJFP2014006)

An analytical method was developed for the simultaneous determination of 32 pesticides including organophosphorus, organochlorine, pyrethroid and carbamate pesticides in fruits and vegetables using gas chromatography-mass spectrometry (GC-MS). The sample was extracted with acetonitrile, and the organic layer was cleaned up with ENVI-Carb and LC-NH₂ cartridges. A large volume of 20 μL purified solution was injected into the GC system using programmable temperature vaporizer (PTV). The mass spectrometric detection was operated with full scan mode. The automated mass spectral deconvolution and identfication system (AMDIS) and an isotopic internal standard were used for the qualitative and quantitative determination of the 32 pesticides, respectively. The conditions for PTV-large volume injection were studied. Furthermore, the selectivity and durability of the method were also assessed. Under the optimized conditions, the experimental results showed that all the linearities were good within their test ranges, with correlation coefficients more than 0.995, and the method detection limits of the pesticides were 2.0-5.0 μg/kg. The spiked recoveries (n=6) at three levels in the 0.010-0.50 mg/kg using spinach, snap bean and cucumber samples as blank matrices were in the range of 65.2%-120.3% with the relative standard deviations (RSDs) varying from 4.1% to 22.3%, showing good accuracy of the method. The advantages of the proposed method include high throughput, high sensitivity, reliability, robustness, and the ability to meet the demand of multi-residue pesticide analysis in fruits and vegetables.
1. [1]
  [1] Cui S H, Chen W S, Qian J L, et al. Chinese Journal of Chromatography (崔淑华, 陈慰双, 钱家亮, 等. 色谱), 2013, 31(9): 885
2. [2]
  [2] Ramírez Restrepo A, Gallo Ortiz A F, Hoyos Ossa D E, et al. Food Chem, 2014, 158: 153
3. [3]
  [3] Lian Y J, Pang G F, Shu H R, et al. J Agric Food Chem, 2010, 58(17): 9428
4. [4]
  [4] Ruan H, Rong W G, Ma Y J, et al. Chinese Journal of Chromatography (阮华, 荣维广, 马永建, 等. 色谱), 2013, 31(12): 1211
5. [5]
  [5] Ding L P, Cai C P, Wang D H. Chinese Journal of Chromatography (丁立平, 蔡春平, 王丹红. 色谱), 2014, 32(8): 849
6. [6]
  [6] Chen B, Jin B, Jiang R, et al. Anal Methods, 2014, 6(6): 1743
7. [7]
  [7] Fu L, Liu Z S, Sun X Y, et al. Scientia Agricultura Sinica (付蕾, 刘正生, 孙鑫洋, 等. 中国农业科学), 2010, 43(21): 4473
8. [8]
  [8] Wu L, Liu W, Cao J, et al. Anal Methods, 2013, 5(5): 1259
9. [9]
  [9] Mallard W G. Anal Bioanal Chem, 2014, 406(21): 5075
10. [10]
  [10] Lu D, Yang Y, Luo X, et al. Anal Methods, 2013, 5(7): 1721
11. [11]
  [11] Zhou J, Wang S Y, Chang Y W, et al. Chinese Journal of Chromatography (周佳, 王霜原, 常玉玮, 等. 色谱), 2012, 30(10): 1037
12. [12]
  [12] Welter J, Meyer M R, Kavanagh P, et al. Anal Bioanal Chem, 2014, 406(7): 1957
13. [13]
  [13] Serrano M, Silva M, Gallego M. Anal Chim Acta, 2013, 784: 77
14. [14]
  [14] Ahumada D, Guerrero J. Vitae, 2013, 20(3): 184
15. [15]
  [15] Banerjee K, Patil S H, Dasgupta S, et al. J Chromatogr A, 2008, 1190(1): 350
16. [16]
  [16] Anastassiades M, Lehotay S J, Stajnbaher D, et al. J AOAC Int, 2003, 86(2): 412
17. [17]
  [17] GB/T 19648-2006
18. [18]
  [18] Norli H R, Christiansen A, Holen B. J Chromatogr A, 2010, 1217(13): 2056
19. [19]
  [19] European Commission. Document No. SANCO/12571/2013 Method Validation & Quality Control Procedures for Pesticide Residues Analysis in Food & Feed. (2014-01-01) [2014-08-28]. http://www.eurl-pesticides.eu/library/docs/allcrl/AqcGuidance_Sanco_2013_12571.pdf
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