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目的建立固相萃取-高效液相色谱测定蔬菜中多菌灵残留量的方法,为了解食品污染及有害因素监测提供技术支持。方法样品中多菌灵用1%乙酸-乙腈溶液提取,上清液经PCX固相萃取柱净化,洗脱液经吹干后用流动相稀释,经0.45μm滤膜过滤后上机测定。经Waters SunFireTMC18色谱柱(250 mm×4.6 mm,5μm)分离,以乙腈-10 mmol/L乙酸铵溶液(30∶70,V/V)为流动相,流速为1.0 ml/min,柱温35℃,利用二极管阵列(PDA)检测器检测,检测波长为286 nm,外标法定量。结果在0.10 mg/L~4.0 mg/L范围内,多菌灵的峰面积与其浓度呈线性相关,相关系数为0.9999,方法检出限为0.020 mg/kg,平均加标回收率为88%~107%,相对标准偏差为2.0%~5.7%。结论本方法前处理简单、快速,检测结果准确、可靠、方法选择性强、灵敏度高,适合于蔬菜中多菌灵残留量的测定。
Objective To establish a method for the determination of carbendazim residues in vegetables by solid-phase extraction and high performance liquid chromatography (HPLC), and provide technical support for the monitoring of food contamination and harmful factors. Methods The carbendazim was extracted with 1% acetic acid-acetonitrile solution. The supernatant was purified by PCX solid-phase extraction. The eluate was diluted with mobile phase after drying and filtered through 0.45 μm membrane filter. The reaction mixture was separated on a Waters SunFire TM C18 column (250 mm × 4.6 mm, 5 μm) using acetonitrile-10 mmol / L ammonium acetate solution (30:70, V / V) as the mobile phase at a flow rate of 1.0 ml / , Using a diode array (PDA) detector detection, detection wavelength of 286 nm, external standard quantitative. Results In the range of 0.10 mg / L to 4.0 mg / L, the peak area of carbendazim was linearly correlated with its concentration, the correlation coefficient was 0.9999, the detection limit was 0.020 mg / kg and the average recovery was 88% 107%, the relative standard deviation was 2.0% ~ 5.7%. Conclusion The method has the advantages of simple and rapid pre-treatment, accurate and reliable detection results, strong selectivity and high sensitivity, and is suitable for the determination of carbendazim residues in vegetables.