UPLC-MS/MS与HPLC测定茶叶中10种氨基甲酸酯类农药残留的比较

比较了超高效液相色谱-串联质谱（UPLC-MS/MS）与高效液相色谱（HPLC）法测定茶叶中10种氨基甲酸酯类农药残留的分析方法。样品经乙腈提取,氨基固相萃取柱净化,HPLC和UPLC-MS/MS测定。结果表明,在相同的前处理条件下,两种方法均具有较好的准确度和精密度,UPLC-MS/MS法在0.01⁰.1mg/kg添加水平下回收率为75.2%¹15.6%,相对标准偏差（RSD）为4.4%¹6.7%。HPLC法在0.05¹.0mg/kg添加水平下回收率为82.7%¹20.7%,相对标准偏差（RSD）为0.8%¹2.9%。UPLC-MS/MS法相对于HPLC法有更高的灵敏度,10种氨基甲酸酯类农药在UPLC-MS/MS上检出限为0.02⁰.3μg/kg,HPLC法检出限为3⁷.5μg/kg;其高灵敏度和选择性,使其更适于多农药残留同时检测和微量残留检测。 

Comparison of UPLC-MS/MS and HPLC for determination of 10 carbamate pesticide residues of tea

The ultra performance liquid chromatography-tandem mass spectrometry (UPLC-MS/MS) and high performance liquid chromatography (HPLC) for determination of 10 carbamate pesticide residues of tea were compared. The samples were extracted with acetonitrile, and cleaned up by amino solid-phase extraction column, then determined by HPLC and UPLC- MS / MS. The results showed that, both methods had good accuracy and precision. The recoveries ranged 75.2%¹15.6% by UPLC-MS/MS when spiked levels 0.01⁰.1mg/kg, with the relative standard deviations 4.4% ¹6.7%. The recoveries ranged 82.7% ¹20.7% by HPLC when spiked levels 0.05¹.0mg/kg, with the relative standard deviations 0.8%¹2.9%. UPLC-MS/MS had higher sensitivity, compared to HPLC, LOD of 10 carbamate pesticides on UPLC-MS/MS was 0.02⁰.3μg/kg, which on HPLC was 3⁷.5μg/kg. UPLC-MS/MS was more suitable for detection of multiple pesticide residues and trace pesticides because its high sensitivity and selectivity.