School of Chemical and Biological Engineering, University of Science and Technology Beijing, Beijing 100083, China.
Bull Environ Contam Toxicol. 2011 Oct;87(4):448-51. doi: 10.1007/s00128-011-0383-z. Epub 2011 Aug 11.
A rapid, sensitive and reliable analytical method for thidiazuron residues in apple and soil was established. The residual levels of the pesticide in apple and soil were determined by high performance liquid chromatography (HPLC) with UV detector. Samples of apple and soil were extracted with acetonitrile-water solutions, and then cleaned up by Florisil or C(18) cartridges. The results showed good linearity (r(2)=1.000) over the concentration range of 0.01-5.0 mg/L. Limits of quantification (LOQ) of the method were 0.01 mg/kg for both soil and apple. Recovery from the apple and soil samples were 83.36%-84.08% and 85.27%-89.83%, respectively, and the corresponding relative standard deviations (RSDs) of the recovery data were 0.155%-0.524% and 0.475%-4.79% for the three fortified levels (0.01, 0.1, 0.5 mg/kg). The analyte in the samples were further confirmed by electrospray ionization tandem mass spectrometry (ESI-MS/MS). It was demonstrated that the proposed method was simple and efficient, and particularly suitable for detecting thidiazuron residues in apple and soil.
建立了一种快速、灵敏、可靠的测定苹果和土壤中噻苯隆残留的分析方法。采用高效液相色谱-紫外检测器（HPLC-UV）法对苹果和土壤中的噻苯隆残留量进行检测。样品经乙腈-水提取，弗罗里硅土或 C(18)柱净化后，用 HPLC-UV 进行测定。结果表明，在 0.01-5.0 mg/L 浓度范围内，噻苯隆残留量与峰面积呈良好的线性关系（r(2)=1.000）。方法的检出限（LOQ）为 0.01 mg/kg（土壤和苹果）。在苹果和土壤中的加标回收率为 83.36%-84.08%和 85.27%-89.83%，相对标准偏差（RSD）为 0.155%-0.524%和 0.475%-4.79%（三个加标水平：0.01、0.1、0.5 mg/kg）。采用电喷雾串联质谱法（ESI-MS/MS）对样品中的分析物进行确证。结果表明，该方法简单、高效，特别适用于苹果和土壤中噻苯隆残留的检测。
