蜂蜜中杀虫脒残留量检验方法研究

Study on determination method of chlordimeform residue in honey

研究了蜂蜜中杀虫脒残留量的测定方法。在丙酮氢氧化钠溶液中以正己烷提取杀虫脒,提取液经碱-正己烷、酸-正己烷液-液分配法净化后,采用气相色谱质谱联用仪(gas chromatography-mass spectrometry, GC-MS)进行定性和定量分析。当标准品质量浓度为0.005~2.000μg/mL时,相关系数r=0.999 3,方法的检出低限为0.002 mg/kg,加标回收率为96.9%~101.8%,变异系数为1.83%~4.03%。方法相对于国标,处理更为简便,且未降低灵敏度,重复性好,准确可靠,可作为检测机构日常蜂蜜中杀虫脒的检测方法进行推广。

A method for the determination of chlordimeform residues in honey was studied. Chlordimeform was extracted with n-hexane in acetone sodium hydroxide solution. After purification by alkali-n-hexane and acid-n-hexane liquid-liquid distribution method, the extract was analyzed qualitatively and quantitatively by gas chromatography-mass spectrometry(GC-MS). When the mass concentration of the standard was 0.005 ~ 2.000 μg/mL, the correlation coefficient was r=0.999 3, the detection limit of the method was 0.002 mg/kg, the recovery was 96.9 % ~ 101.8 %, and the coefficient of variation was 1.83 % ~ 4.03 %. Compared with the national standard, the method has the advantages of simpler treatment, no reduction in sensitivity, good repeatability, accuracy and reliability. It can be popularized as the detection method of chlordimeform in daily honey of detection institutions.