论文部分内容阅读
建立了气相色谱-四极杆-飞行时间质谱同时筛查食品中182种香港《食物内残余除害剂规例》农药残留的分析方法。样品经含0.1%(v/v)甲酸的乙腈溶液提取,改进的QuEChERS方法净化,采用Agilent HP-5MS色谱柱(30 m×0.25 mm×0.25μm)进行分离。样品经电子轰击源电离,一级质谱采用全扫描模式完成化合物的定性和定量检测,对疑似物质进行二级谱库检索确证。考察了10种典型食品基质(大米、香菇、黄豆、菠菜、西红柿、西兰花、柚子、胡萝卜、生菜、黄瓜)的基质效应。在10~500μg/kg范围内,182种目标化合物的线性关系良好(r>0.99),方法的定量限(S/N≥10)为10~100μg/kg,在3个添加水平下的平均加标回收率分别为66.1%~121.5%、75.4%~125.8%、77.2%~128.9%,相对标准偏差(RSD)为0.8%~17.6%(n=6)。该方法操作简单、耗时短、灵敏度高、稳定性好,可显著降低日常筛查检测的成本,具有实际应用价值。
A gas chromatography-quadrupole-time of flight mass spectrometry (GC-MS / MS) method was developed for simultaneous determination of 182 pesticide residues in foodstuffs in Hong Kong’s Residual Pesticides in Food Regulations. Samples were extracted with acetonitrile containing 0.1% (v / v) formic acid, purified by a modified QuEChERS method and separated on an Agilent HP-5MS column (30 m × 0.25 mm × 0.25 μm). The sample was ionized by electron bombardment, and the first-order mass spectrometry was used to perform the qualitative and quantitative detection of the compound with the full-scan mode. The secondary substance library was searched to confirm the suspected substance. The matrix effects of 10 typical food matrices (rice, shiitake, soy, spinach, tomato, broccoli, grapefruit, carrot, lettuce, cucumber) were examined. The linear relationship of 182 target compounds was good (r> 0.99) in the range of 10 ~ 500μg / kg, and the limit of quantification (S / N≥10) was 10 ~ 100μg / kg in the range of 10 ~ 500μg / The standard recoveries ranged from 66.1% to 121.5%, from 75.4% to 125.8% and from 77.2% to 128.9%, respectively. The relative standard deviations (RSDs) ranged from 0.8% to 17.6% (n = 6). The method has the advantages of simple operation, short time-consuming, high sensitivity and good stability, and can obviously reduce the cost of routine screening tests and has practical application value.