Ma Youning, Chen Mingxue, Mou Renxiang, Cao Zhaoyun
China National Rice Research Institute, Hangzhou, Zhejiang, 311400, China.
Rapid Commun Mass Spectrom. 2019 May 15;33(9):867-874. doi: 10.1002/rcm.8409.
The presence of organotins in the environment affects food safety, making it important to monitor the levels of organotin pesticides (OTPs) in fruit and vegetable samples.
In the present study, a simple and low cost method for simultaneous determination of three OTPs (azocyclotin, fenbutatin oxide and triphenyltin hydroxide) in vegetable and fruit samples was developed and validated, based on solid-phase extraction and liquid chromatography/tandem mass spectrometry.
Extraction with acetonitrile containing 0.2% formic acid positively affected the recoveries of the three OTPs. Moreover, the simultaneous purification of the three OTPs was the most efficient using mixed-mode cation-exchange cartridges and 5.0% ammonium hydroxide in methanol as eluent, and, in this case, mild matrix effects (-9.3% to 21.6%) were obtained for the three OTPs monitored. The developed method reached limits of quantification of 1 μg kg , and linearity was satisfactory, with correlation coefficients >0.995. A fortification study showed that when spiked at 1.0-50.0 μg kg the mean trueness values were from 72.3 to 110.0% in all matrices (three vegetables and three fruits). The intra-day precision was <14.1%, and the inter-day precision (n = 11) was <18.2%.
The proposed method was successfully applied to the simultaneous analysis of three OTPs in vegetables and fruits.
环境中有机锡的存在会影响食品安全,因此监测水果和蔬菜样品中有机锡农药(OTP)的含量非常重要。
在本研究中,基于固相萃取和液相色谱/串联质谱法,开发并验证了一种简单且低成本的同时测定蔬菜和水果样品中三种OTP(三环锡、三苯锡和氢氧化三苯基锡)的方法。
用含0.2%甲酸的乙腈萃取对三种OTP的回收率有积极影响。此外,使用混合模式阳离子交换柱和5.0%氢氧化铵的甲醇溶液作为洗脱剂,对三种OTP进行同时净化最为有效,在这种情况下,所监测的三种OTP的基质效应较温和(-9.3%至21.6%)。所开发的方法定量限达到1 μg/kg,线性良好,相关系数>0.995。强化研究表明,在1.0 - 50.0 μg/kg加标时,所有基质(三种蔬菜和三种水果)中的平均真实值在72.3%至110.0%之间。日内精密度<14.1%,日间精密度(n = 11)<18.2%。
所提出的方法成功应用于蔬菜和水果中三种OTP的同时分析。