State Key Laboratory Breeding Base for Zhejiang Sustainable Pest and Disease Control, Institute of Plant Protection and Microbiology, Zhejiang Academy of Agricultural Sciences, Hangzhou 310021, PR China.
J Chromatogr B Analyt Technol Biomed Life Sci. 2013 Feb 1;915-916:13-20. doi: 10.1016/j.jchromb.2012.12.016. Epub 2012 Dec 27.
A simple, sensitive and reliable analytical method was developed for the simultaneous determination of 22 carbamate insecticides and 17 mycotoxins in cereals by ultra high performance liquid chromatography electrospray ionization tandem mass spectrometry (UHPLC-ESI-MS/MS). Carbamates and mycotoxins were extracted from cereal samples using a QuEChERS (Quick, Easy, Cheap, Effective, Rugged and Safe) procedure without any further clean-up step. The extract was diluted with water containing 0.1% formic acid and 5.0mM ammonium acetate, and analyzed by LC-MS/MS on a Waters Acquity BEH C(18) column with water (0.1% formic acid, 0.50mM ammonium acetate)/methanol as mobile phase with gradient elution. Matrix-matched calibration was used for quantification. Blank samples (rice, wheat and corn) were fortified at 5, 10 and 50 μg/kg except for five zearalenonic compounds at 25, 50 and 250 μg/kg, and recoveries were in the range of 70-120%. Relative standard deviations were lower than 20% in all cases. The LOQ values were in the range of 0.20-29.7 μg/kg. The method is suitable for the simultaneous determination of carbamate insecticides and mycotoxins in cereals. The total time required for the analysis of one sample, including sample preparation, was about 35 min.
建立了一种超高效液相色谱-电喷雾串联质谱法（UHPLC-ESI-MS/MS）同时测定谷物中 22 种氨基甲酸酯类杀虫剂和 17 种真菌毒素的分析方法。采用 QuEChERS（快速、简单、廉价、有效、耐用、安全）法从谷物样品中提取氨基甲酸酯类杀虫剂和真菌毒素，无需进一步净化。提取液用含有 0.1%甲酸和 5.0mM 乙酸铵的水稀释，在 Waters Acquity BEH C(18)柱上用含 0.1%甲酸、0.50mM 乙酸铵的水/甲醇作为流动相进行 LC-MS/MS 分析，梯度洗脱。采用基质匹配校准进行定量。空白样品（大米、小麦和玉米）在 5、10 和 50μg/kg 水平进行添加，除了五种玉米赤霉烯酮化合物在 25、50 和 250μg/kg 水平进行添加，回收率在 70-120%范围内。所有情况下，相对标准偏差均低于 20%。LOQ 值在 0.20-29.7μg/kg 范围内。该方法适用于谷物中氨基甲酸酯类杀虫剂和真菌毒素的同时测定。包括样品制备在内，分析一个样品的总时间约为 35 分钟。
