Zhao Li, Chen Guo, Zhao Jian, Zhang Yan, Zhu Yong, Yang Ting, Wu Yin-Liang
Shanghai Agriculture Technical Extension Service Center, Shanghai 201103, PR China.
The Ningbo Academy of Agricultural Sciences, Ningbo 315040, PR China.
Chemosphere. 2015 Jan;119:1185-1191. doi: 10.1016/j.chemosphere.2014.10.026. Epub 2014 Nov 1.
The fate of spinetoram was studied in a rice field ecosystem, and an efficient method for the determination of spinetoram (XDE-175-J and XDE-175-L) in soil, rice straw, paddy water, husk and brown rice was developed. Spinetoram residues were extracted from samples with a salting out extraction procedure. The extracts were diluted with 0.10% formic acid in water and analysed with liquid chromatography tandem mass spectrometry (LC-MS/MS) on a Waters Acquity BEH C18 column. The calibration curve was linear in the range 0.125-100 μg L(-1) and r>0.999. The average recovery was 82.9-89.0% from soil, 78.5-92.1% from rice straw, 93.6-100.3% from paddy water, 79.1-87.9% from brown rice and 72.7-82.9% from husk. The relative standard deviation (RSD) was less than 10%. These results are all within the accepted range for pesticide residue determination. The field test results showed that spinetoram degradation in paddy water, soil and rice straw coincided with C=0.0132e(-1.9685t), C=0.0308e(-0.1018t) and C=0.8530e(-0.6223t), respectively. The half-lives of spinetoram in paddy water, soil and rice straw were 0.35, 6.8 and 1.1 d, respectively. The final residue level was lower than the maximum residue limit (MRL) of 0.05 mg kg(-1) for spinetoram in rice with a harvest interval of 7d. A dosage of 450 mL ha(-1) was recommended, which can be considered safe for human beings and animals. The results of this study will contribute to establishing the scientific basis of the dosage of spinetoram for agricultural fields.
研究了乙基多杀菌素在稻田生态系统中的归宿,并开发了一种测定土壤、稻草、稻田水、稻壳和糙米中乙基多杀菌素(XDE - 175 - J和XDE - 175 - L)的有效方法。采用盐析萃取法从样品中提取乙基多杀菌素残留。提取物用0.10%的甲酸水溶液稀释,然后在Waters Acquity BEH C18柱上用液相色谱串联质谱法(LC - MS/MS)进行分析。校准曲线在0.125 - 100 μg L⁻¹范围内呈线性,r > 0.999。土壤中的平均回收率为82.9 - 89.0%,稻草中的为78.5 - 92.1%,稻田水中的为93.6 - 100.3%,糙米中的为79.1 - 87.9%,稻壳中的为72.7 - 82.9%。相对标准偏差(RSD)小于10%。这些结果均在农药残留测定的可接受范围内。田间试验结果表明,乙基多杀菌素在稻田水、土壤和稻草中的降解分别符合C = 0.0132e⁻¹.⁹⁶⁸⁵ᵗ、C = 0.0308e⁻⁰.¹⁰¹⁸ᵗ和C = 0.8530e⁻⁰.⁶²²³ᵗ。乙基多杀菌素在稻田水、土壤和稻草中的半衰期分别为0.35、6.8和1.1天。收获间隔为7天时,糙米中乙基多杀菌素的最终残留水平低于最大残留限量(MRL)0.05 mg kg⁻¹。建议使用剂量为450 mL ha⁻¹,这对人和动物可认为是安全的。本研究结果将有助于为农田乙基多杀菌素的施用量建立科学依据。