Chen Xiu, Dong Fengshou, Liu Xingang, Xu Jun, Li Jing, Li Yuanbo, Wang Yunhao, Zheng Yongquan
Institute of Plant Protection, Chinese Academy of Agricultural Sciences, Key Laboratory of Pesticide Chemistry and Application, Ministry of Agriculture, Beijing, P. R. China.
J Sep Sci. 2012 Jan;35(2):200-5. doi: 10.1002/jssc.201100823.
An effective chiral analytical method was developed for the resolution and determination of dinotefuran enantiomers in rice, tomato and apple samples. Dinotefuran enantiomers were baseline-separated and determined on a novel chiral column, ChromegaChiral CCA, with n-hexane-ethanol-methanol (85:5:10, v/v/v) as the mobile phase at a flow rate of 1.0 mL/min with UV detection at 270 nm. The resolution of dinotefuran enantiomers was about 1.8. The first eluted enantiomer was (+)-dinotefuran and the second eluted one was (-)-dinotefuran. The effects of mobile-phase composition and column temperature on the enantioseparation were evaluated. The method was validated for linearity, repeatability, accuracy, LOD and LOQ. LOD was 0.15 mg/kg in rice and tomato, 0.05 mg/kg in apple, with an LOQ of 0.5 mg/kg in rice and tomato, 0.2 mg/kg in apple. The average recoveries of the pesticide from all matrices ranged from 75.8 to 92.9% for all fortification levels The precision values associated with the analytical method, expressed as RSD values, were <16.5% for the pesticide in all matrices. The methodology was successfully applied for the enantioselective analysis of dinotefuran enantiomers in real samples, indicating its efficiency in investigating the environmental stereochemistry of dinotefuran in food matrix.
建立了一种有效的手性分析方法，用于分离和测定大米、番茄和苹果样品中的呋虫胺对映体。呋虫胺对映体在新型手性柱ChromegaChiral CCA上实现基线分离并测定，以正己烷 - 乙醇 - 甲醇（85:5:10，v/v/v）为流动相，流速为1.0 mL/min，在270 nm处进行紫外检测。呋虫胺对映体的分离度约为1.8。先洗脱的对映体是(+)-呋虫胺，后洗脱的是(-)-呋虫胺。评估了流动相组成和柱温对映体分离的影响。该方法进行了线性、重复性、准确性、检测限和定量限的验证。大米和番茄中的检测限为0.15 mg/kg，苹果中的检测限为0.05 mg/kg，大米和番茄中的定量限为0.5 mg/kg，苹果中的定量限为0.2 mg/kg。在所有加标水平下，该农药在所有基质中的平均回收率为75.8%至92.9%。与分析方法相关的精密度值，以相对标准偏差（RSD）表示，该农药在所有基质中的RSD值均<16.5%。该方法成功应用于实际样品中呋虫胺对映体的对映选择性分析，表明其在研究食品基质中呋虫胺的环境立体化学方面的有效性。
