QuEChERS-高效液相色谱-串联质谱法快速测定罗汉果中55种杀菌剂

建立了广西名优特产罗汉果中55种杀菌剂残留的QuEChERS-高效液相色谱-串联质谱(HPLC-MS/MS)检测方法。试样经1%(v/v)醋酸乙腈提取后,加入无水硫酸镁脱水,并使用无水硫酸钠、N-丙基乙二胺(PSA)和C18进行净化。采用均含有0.005 mol/L甲酸铵及0.01%(v/v)甲酸的95%(v/v)乙腈水溶液和水作为流动相中的有机相和水相进行梯度洗脱,在电喷雾离子源正离子模式(ESI+)下采用动态多反应监测(DMRM)进行扫描,基质匹配外标法定量。55种杀菌剂在1.0~100.0μg/kg范围内线性相关性良好,相关系数(R~2)0.99;方法的检出限(S/N3)为1.0μg/kg,定量限(S/N10)为10.0μg/kg;加标(10.0μg/kg)回收率为76.96%~118.45%,相对标准偏差为3.44%~19.63%(n=6)。该法快速、准确、灵敏,适合高通量检测罗汉果中的杀菌剂残留。

Rapid determination of 55 fungicides in siraitia grosvenoriis by QuEChERS and high performance liquid chromatography-tandem mass spectrometry

A method for the determination of 55 fungicides in siraitia grosvenoriis by QuEChERS and high performance liquid chromatography-tandem mass spectrometry (HPLC-MS/MS) was established. The samples were extracted with acetonitrile containing 1%(v/v) acetic acid, then dehydrated by anhydrous magnesium sulfate and purified by anhydrous sodium sulfate, N-propyl ethylenediamine (PSA) and C18. Then, 95% (v/v) acetonitrile aqueous solution (organic phase) and water (aqueous phase), both containing 0.005 mol/L ammonium formate and 0.01% (v/v) formic acid, were used as mobile phases with gradient elution. The compounds were tested by positive electrospray ion source (ESI⁺) and dynamic multiple reaction monitoring (DMRM) mode. Fifty-five fungicides were quantified by external standard method considering matrix effects. The correlation coefficients (R²) were greater than 0.99, which indicated that the linear dependence of the 55 fungicides were good in the range of 1.0-100.0 μg/kg. The LODs (S/N>3) and LOQs (S/N>10) of all the fungicides were 1.0 μg/kg and 10.0 μg/kg, respectively. The recoveries were in the range of 76.96%-118.45% and the relative standard deviations (RSDs) ranged from 3.44% to 19.63% (n=6). This method has the advantages of rapidity, accuracy and sensitivity for the high-throughput detection of fungicides residues in siraitia grosvenoriis.