气相色谱-三重四级杆质谱法同时测定野生黄精中27种农残

Determination of 27 kinds of pesticide residues in wild rhizoma polygonati by GC-MS

建立了气相色谱-三重四级杆质谱法(gas chromatography-triple quadruple mass spectrometry,GC-MS/MS)测定黄精中27种农残的定量分析方法。采用三重四极杆质谱的选择性反应监测技术(SRM)对27种农残的特征离子和碰撞能量进行优化,确定最佳质谱条件。为避免基质效应,采用空白基质配制标准溶液。结果表明,待测农残在线性范围(5~500 ng/mL)内呈现良好的线性关系,线性系数均大于0.995(R:0.9976~0.9998),检出限为0.003~0.014 mg/kg,定量限为0.010~0.040 mg/kg,加标回收率为82.6~107.3%。该方法具有用时短、灵敏度高、选择性好的优点,可用于大批量黄精样品的多项农残检测。

The selective reaction monitoring technology(SRM)of triple quadrupole mass spectrometry was used to optimize the characteristic ions and collision energy of 27 kinds of pesticide residues and determine the optimal mass spectrometry conditions. In order to avoid matrix effect,blank matrix was used to prepare standard solution. The results showed that there was a good linear relationship within the linear range of 5—500 ng/mL for the pesticide residues to be tested. The linear coefficients were all greater than 0. 995(R:0. 9976— 0. 9998). The detection limit was 0. 003— 0. 014 mg/kg,the quantitative limit was 0. 010—0. 040 mg/kg,and the spiked recovery rates was 82. 6%—107. 3%. The method has the advantages of short time,high sensitivity and good selectivity,and can be used for the detection of multiple pesticide residues in large quantities of samples.