Application of QuEchERS Method in Determining Imidaclothiz Residue in Soil and Citrus by Ultra-Performance Liquid Chromatography Tandem Mass Spectrometry

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Abstract:

A simple method for the determination of imidaclothiz residue in soil and citrus samples was established by ultra-performance liquid chromatography tandem mass spectrometry (UPLC-MS/MS) under the multiple reaction monitoring (MRM) mode. Imidaclothiz was extracted from soil and citrus samples using a procedure known as the quick, easy, cheap, effective, rugged, and safe (QuEChERS) method. Experiments on 3 fortification concentrations were carried out, and the limit of determination is 1.0×10-10 g. The recoveries ranging from 80.7% to 118.9% with high correlation coefficient (r>0.99) were obtained within the linear range (0.01-1.0mg/kg). Based on the above method, we also carried out field trials. Results showed that the degradation of imidaclothiz coincided with the fitted equations Ct=0.1028e-0.0266t, Ct=0.1778e-0.0311t in soil and Ct=1.3612e-0.0632t, Ct=0.7162e-0.0968t in citrus, respectively, with the average half-lives of 24.2 d in soil and 9.1 d in citrus, respectively. The results indicate that the developed method is fast, accurate, and easy to operate. It also demonstrates that the method can meet the requirements of determination of imidaclothiz in soil and citrus.

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Advanced Materials Research (Volumes 343-344)

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855-861

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September 2011

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© 2012 Trans Tech Publications Ltd. All Rights Reserved

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[1] 67 41.

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[42] 2.

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[57] 8 hangzhou clay.

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[5] 82.

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[1] 94 37.

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[41] 5.

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[58] 5 wuhan loamy clay.

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[6] 74.

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[2] 92 34.

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[61] 6.

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[38] 4 quanzhou loam.

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[6] 43.

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578 38.

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[32] 1.

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[67] 9 haerbing loam.

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[8] 06.

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[2] 62 46.

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[24] 7.

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[75] 3 hefei silty clay.

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[1] 32 33.

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[59] 1 TABLE I. Fortified recovery of the method for imidaclothiz residue in soil and orange samples Field area and sample type Fortified concentration (mg/kg).

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1 1 (X±S) (%) n=3 CV (%) (X±S) (%) n=3 CV (%) (X±S) (%) n=3 CV (%) chengdu soil 105. 9±6. 6.

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[6] 2 112. 0±7. 4.

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[6] 6 108. 5±3. 6.

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[3] 3 hangzhou soil 100. 7±1. 1.

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[98] 1±.

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[3] 4 104. 5±4. 2.

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[4] 0 wuhan soil.

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[91] 3±.

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[3] 9 101. 3±4. 0.

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[3] 9 118. 5±6. 1.

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[5] 1 quanzhou soil 116. 0±13. 9.

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[11] 9 109. 8±4. 7.

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[4] 3 112. 8±3. 9.

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[3] 5 haerbing soil.

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[87] 4±.

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[8] 5 101. 4±2. 0.

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[2] 0 107. 7±4. 9.

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[4] 5 hefei soil 110. 0±7. 8.

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[7] 1 102. 6±3. 2.

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[3] 1 104. 2±5. 8.

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[5] 6 quzhou soil.

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[86] 7±.

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[92] . 6±.

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[96] 7±.

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[4] 7 quzhou orange.

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[87] 2±.

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[92] 6±.

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[93] 6±.

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[4] 3 dongshan soil.

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[80] 7±.

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[5] 7 100. 4±3. 8.

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[3] 8 115. 3±5. 5.

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[4] 8 dongshan orange.

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[88] 9±.

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[98] 5±.

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[6] 7 100. 8±3. 7.

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[3] 7 x-average recoveries s-standard deviation cv-coefficient of variation Figure 1. The chromatogram of the selection of the first daughter ion and its optimal energy Figure 2. The chromatogram of the selection of the second daughter ion and its optimal energy Figure 3. Representative chromatogram of (a) standard of imidaclothiz, (b) soil blank, (c) soil blank spiked with standard of imidaclothiz, (d) soil sample with imidaclothiz residue, (e) citrus blank, (f) citrus blank spiked with standard of imidaclothiz, (g) citrus sample with imidaclothiz residue. Figure 4. The degradation dynamics of imidaclothiz in soil and citrus.

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