Abstract
An analytical method for the simultaneous determination of 19 kinds of organochlorine pesticides in apple-pear was established based on optimized solid-phase extraction coupled with gas chromatography-mass spectrometry（SPE-GC/MS）. Different extraction conditions, included extraction solvent, extraction solvent volume, sample weight, solid phase extraction clean-up and eluent were optimized during the sample pretreatment. The quantification were analyzed by GC/MS in selected ion monitoring （SIM） mode and the external standard method. The method showed good linearity (R2≥0.996 7) for all the pesticides. The recoveries at three spiked levels (20, 40, and 200 μg/kg) ranged from 86.1% to 108.9% with the relative standard deviation below 10%. The limit of detection ranged from 3 to 6 μg/kg and the limit of quantification ranged from 10.0 to 20.0 μg/kg the for 19 kinds of pesticides, respectively. The method was simple, accurate and showed high sensitivity for screening and detection of the 19 kinds of pesticides in apple-pear.
Publication Date
12-28-2019
First Page
87
Last Page
95
DOI
10.13652/j.issn.1003-5788.2019.12.016
Recommended Citation
Yunheng, YAO; Longlü, BAI; Lunpeng, WU; Xinzi, WU; Tao, YI; Zhenning, QIN; and Xiuli, REN
(2019)
"Determination of 19 kinds of organchlorine pesticide residues in apple-pear by using gas chromatography-mass spectrometry coupled with solid-phase extraction,"
Food and Machinery: Vol. 35:
Iss.
12, Article 16.
DOI: 10.13652/j.issn.1003-5788.2019.12.016
Available at:
https://www.ifoodmm.cn/journal/vol35/iss12/16
References
[1] ALAMGIR Z C, FAKHRUDDIN A, NAZRUL I, et al. Detection of the residues of nineteen pesticides in fresh vegetable samples using gas chromatography-mass spectrometry[J]. Food Control, 2013, 34(2): 457-465.
[2] ANA M, MARIA M S, AGUSTIN L G, et al. Determination of pesticides and veterinary drug residues in food by liquid chromatography-mass spectrometry: A review[J]. Analtica Chimica Acta, 2016, 936: 40-61.
[3] CAO Ya-lian, TANG Hua, CHEN Da-zhou, et al. A novel method based on MSPD for simultaneous determination of 16 pesticide residues in tea by LC-MS/MS[J]. Journal of Chromatography B, 2015, 998/999: 72-75.
[4] CHEN Lei, CHEN Jin-fa, GUO Ying, et al. Study on the simultaneous determination of seven benzoylurea pesticides in Oolong tea and their leaching characteristics during infusing process by HPLC-MS/MS[J]. Food Chemistry, 2014, 143: 405-410.
[5] DIPAKSHI S, AVINASH N, YOGESH B, et al. Analytical methods for estimation of organophosphorus pesticide residues in fruits and vegetables: A review[J]. Talanta, 2010, 82(4): 1 077-1 089.
[6] GEVANY P P, ANTONIO A N, MARIA E L, et al. Optimization of the liquid-liquid extraction method and low temperature purification (LLE-LTP) for pesticide residue analysis in honey samples by gas chromatography[J]. Food Control, 2010, 21(10): 1 307-1 311.
[7] GUAN Wen-bi, LI Zhou-nan, ZHANG Hong-yan, et al. Amine modified graphene as reversed-dispersive solid phase extraction materials combined with liquid chromatography-tandem mass spectrometry for pesticide multi-residue analysis in oil crops[J]. Journal of Chromatography A, 2013, 1 286: 1-8.
[8] GUAN Ya-qian, TANG Hua, CHEN Da-zhou, et al. Modified QuEChERS method for the analysis of 11 pesticide residues in tea by liquid chromatography-tandem mass spectrometry[J]. Analytical Methods, 2013, 5(12): 3 056-3 067.
[9] HAN Yong-tao, SONG Le, ZOU Nan, et al. Multi-residue determination of 171 pesticides in cowpea using modified QuEChERS method with multi-walled carbon nanotubes as reversed-dispersive solid-phase extraction materials[J]. Journal f Chromatography B, 2016, 1 031: 99-108.
[10] HERNANDEZ F, CERVERA M I, PORTOLES T, et al. The role of GC-MS/MS with triple quadrupole in pesticide residue analysis in food and the environment[J]. Analytical Methods, 2013, 5(21): 5 875-5 894.
[11] HOU Xue, LEI Shao-rong, GUO Ling-an, et al. Optimization of a multi-residue method for 101 pesticides in green tea leaves using gas chromatography-tandem mass spectrome-try[J]. Revista Brasileirade Farmacognosia, 2016, 26(4): 401-407.
[12] IGNACIO M, NATALIA G, MARIELA P, et al. Determination of pesticide residues in globe artichoke leaves and fruits by GC-MS and LC-MS/MS using the same QuEChERS procedure[J]. Food Chemistry, 2017, 227: 227-236.
[13] IRINA T, ANDREY S, DARIA K, et al. On-line in-syringe sugaring-out liquid-liquid extraction coupled with HPLC-MS/MS for the determination of pesticides in fruit and berry juices[J]. Talanta, 2017, 167: 761-767.
[14] KUANG Ying, QIU Feng, KONG Wei-jun, et al. Simultaneous quantification of mycotoxins and pesticide residues in ginseng with one-step extraction using ultra-high performance liquid chromatography-electrospray ionization tandem mass spectrometry[J]. Journal of Chromatography B, 2013, 939: 98-107.
[15] LUKMAN B A, GUAN H T. Chemometric approach to the optimization of HS-SPME/GC-MS for the determination of multiclass pesticide residues in fruits and vegetables[J]. Food Chemistry, 2015, 177: 267-273.
[16] MOHD M S, SYAIRAH S, WAN A W I, et al. Molecu-larly imprinted polymer solid-phase extraction for the analysis of organophosphorus pesticides in fruit samples[J]. Journal of Food Composition Analysis, 2013, 32(2): 155-161.
[17] NORMA P F, SILVIA C M, ROBERTO M V, et al. Direct immersion single drop micro-extraction method for multi-class pesticides analysis in mango using GC-MS[J]. Food Chemistry, 2017, 237: 30-38.
[18] RADU C D, GUILLAUME S, EMILIE H, et al. Comparison of solid phase- and liquid/liquid -extraction for the purification of hair extract prior to multi-class pesticides analysis[J]. Journal of Chromatography B, 2014, 955/956: 98-107.
[19] XIE Wen, HAN Chao, QIAN Yan, et al. Determination of neonicotinoid pesticides residues in agricultural samples by solid-phase extraction combined with liquid chromatogra-phy-tandem mass spectrometry[J]. Journal of Chromatography A, 2011, 1 218(28): 4 426-4 433.
[20] YANG Xue, ZHANG Hua, LIU Yan, et al. Multiresidue method for determination of 88 pesticides in berry fruits using solid-phase extraction and gas chromatography-mass spectrometry: Determination of 88 pesticides in berries using SPE and GC-MS[J]. Food Chemistry, 2011, 127(2): 855-865.
[21] ZHANG Ming-lu, CHEN Hong-ping, ZHU Li, et al. Solid-phase purification and extraction for the determination of trace neonicotinoid pesticides in tea infusion[J]. Journal of Separation Science, 2016, 39(5): 910-917.