Yi Xionghai, Han Li, Yang Huiqin, Fan Xiang, Zhu Jian, Guo Dehua
Shanghai Entry-Exit Inspection and Quarantine Bureau, Shanghai 200135, China.
Se Pu. 2010 Jul;28(7):649-53. doi: 10.3724/sp.j.1123.2010.00649.
A liquid chromatography-tandem mass spectrometry (LC-MS/MS) method was developed for the determination of chlordimeform and its metabolite (4-chloro-o-toluidine) residue in acacia honey, chaste honey, comb honey, multifloral honey and wild honey. The samples were dissolved and diluted with sodium hydroxide solution, and cleaned up by a Waters Oasis HLB solid phase extraction column. The separation was performed on an Agilent XDB-C18 column with gradient elution using 0.1% formic acid solution and acetonitrile. The residues of chlordimeform and its metabolite were determined by electrospray ionization-tandem mass spectrometry, and quantified by the method of matrix-matched external standard. The calibration curves for chlordimeform and its metabolite showed good linearity in the range of 2.5 - 250 microg/L with the correlation coefficients (r) higher than 0.999. The limit of quantification was 5 microg/kg, and the limit of detection was 2.5 microg/kg. The recoveries of chlordimeform and 4-chloro-o-toluidine in honey at the spiked levels of 5, 10 and 20 microg/kg were in the ranges of 75.8% - 113.8% and 85.6% - 114.3%, respectively. The relative standard deviations were 4.8% - 10.2% and 4.7% -9.1%, respectively. The method can meet the requirements for the determination of chlordimeform and 4-chloro-o-toluidine in honey for import and export inspection.
建立了一种液相色谱 - 串联质谱（LC-MS/MS）法，用于测定相思蜂蜜、圣洁蜂蜜、巢蜜、多花蜂蜜和野生蜂蜜中杀虫脒及其代谢物（4-氯邻甲苯胺）的残留量。样品用氢氧化钠溶液溶解并稀释，然后通过Waters Oasis HLB固相萃取柱进行净化。采用Agilent XDB-C18柱，以0.1%甲酸溶液和乙腈进行梯度洗脱分离。杀虫脒及其代谢物的残留量通过电喷雾电离 - 串联质谱测定，并采用基质匹配外标法进行定量。杀虫脒及其代谢物的校准曲线在2.5 - 250μg/L范围内呈良好线性，相关系数（r）高于0.999。定量限为5μg/kg，检测限为2.5μg/kg。在5、10和20μg/kg加标水平下，蜂蜜中杀虫脒和4-氯邻甲苯胺的回收率分别在75.8% - 113.8%和85.6% - 114.3%范围内。相对标准偏差分别为4.8% - 10.2%和4.7% - 9.1%。该方法可满足进出口检验中蜂蜜中杀虫脒和4-氯邻甲苯胺测定的要求。
