Residue of pyriminobac-methyl in rice and environment
Received:January 07, 2019    Download the full
DOI：10.16801/j.issn.1008-7303.2019.0035
Key Words:pyriminobac-methyl  rice  residue  QuEChERS  high-performance liquid chromatography-tandem mass spectrometry (HPLC-MS)
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Author NameAffiliationE-mail
JIA Haoran College of Land Resources and Environment, Jiangxi Agricultural University, Nanchang 330045, China  
ZHANG Yue College of Land Resources and Environment, Jiangxi Agricultural University, Nanchang 330045, China  
LI Wei College of Land Resources and Environment, Jiangxi Agricultural University, Nanchang 330045, China  
LI Baotong College of Land Resources and Environment, Jiangxi Agricultural University, Nanchang 330045, China libt66@163.com 
SHI Xugen College of Land Resources and Environment, Jiangxi Agricultural University, Nanchang 330045, China  
TANG Limei College of Land Resources and Environment, Jiangxi Agricultural University, Nanchang 330045, China  
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Abstract:
      A method was developed for the determination of pyriminobac-methyl residues in rice and environment by high-performance liquid chromatography-tandem mass spectrometry (HPLC-MS) coupled with modified QuEChERS. The samples were extracted with a solvent mixture, V (acetonitrile):V (formic acid)=199:1, and then purified by octadecylsilane bonded silica (C18) or C18 + primary secondary amine (PSA) adsorbents. The analytes were separated on a ZORBAX SB C18 column using a solvent mixture, V (acetonitrile):V (0.1% formic acid aqueous solution)=70:30, as mobile phase. Pyriminobac-methyl was detected by HPLC-MS with an electrospray ionization source (ESI+) in positive mode. Quantization was performed using external standard method. The results showed good linear relationship between the peak area of pyriminobac-methyl and its mass concentration in the range from 0.01 mg/L to 1 mg/L. And the correlation coefficients in acetonitrile, paddy water, soil, rice stalk, brown rice and rice husk were all above 0.99. The limit of detection (LOD) for pyriminobac-methyl was 0.0015 mg/L in paddy water, while the limit of quantification (LOQ) was 0.005 mg/L. The LOD were 0.003, 0.015, 0.015 and 0.003 mg/kg in soil, brown rice, rice hull and rice stalk, respectively, while the corresponding LOQ were 0.01, 0.05, 0.05 and 0.01 mg/kg, respectively. The average spiked recoveries of pyriminobac-methyl at three spiked levels of 0.005, 0.01 and 0.1 mg/L (or mg/kg) in paddy water, soil and brown rice were 95%-109%, 92%-106% and 89%-107%, respectively, with the relative standard deviation (RSD) of 3.0%-5.0%, 1.1%-2.9% and 3.1%-3.7%, respectively. The average spiked recoveries in rice hull and rice stalk were 95%-102% and 93%-107%, respectively, with the RSD of 1.1%-3.8% and 3.5%-9.9%, respectively. The sensitivity, precision and accuracy of the method meet the requirements of pesticide residue analysis.
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