LC-MS/MS法测定桑叶药材中100种农药残留量
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篇名: LC-MS/MS法测定桑叶药材中100种农药残留量
TITLE:
摘要: 目的:建立测定桑叶药材中100种农药残留量的方法。方法:采用液相色谱-串联质谱法(LC-MS/MS)。色谱条件:色谱柱为ZORBAX Eclipse plus C18,流动相为乙腈(含5%水、0.1%甲酸、5 mmol/L甲酸铵)-水(含0.1%甲酸、5 mmol/L甲酸铵)(梯度洗脱),流速为0.4  ml/min,柱温:40 ℃;进样量:5 μl;质谱条件:电离源为电喷雾离子源,正离子模式,扫描方式为动态MRM,扫描时间窗为2 min;雾化气为氮气,雾化气压为40 psi,干燥气流速为5 L/min,毛细管电压为4 000 V,离子喷雾电压为500 V。结果:100种农药检测质量浓度线性范围均为2.4~150 ng/ml(r>0.990 0),加样回收率范围均为69.3%~128.2%,各农药的方法检测限范围为0.003~16 μg/kg。结论:该方法操作简便、快速、灵敏度高,可用于桑叶药材中多种农药残留量的测定。
ABSTRACT: OBJECTIVE: To establish a method for the determination of 100 pesticide residues in Morus alba. METHODS: LC-MS/MS was conducted on the column of ZORBAX Eclipse plus C18 with mobile phase of acetonitrile (containing 5% water, 0.1% formic acid, 5 mmol/L ammonium formate) - water (containing 0.1% formic acid, 5 mmol/L ammonium formate) (gradient elution) at a flow rate of 0.4 ml/min, column temperature was 40 ℃, injection volume was 5 μl; MS conditions: ionization source was electrospray ionization with positive ion mode, scanning mode was dynamic MRM, scanning time window was 2 min; atomizing gas was nitrogen, atomizing gas pressure was 40 psi, drying gas flow rate was 5 L/min, capillary voltage was 4 000 V, and ion spray voltage was 500 V. RESULTS: The linear range of 100 pesticide residues was 2.4-150 ng/ml (r>0.990 0), recovery was 69.3%-128.2%, and the determination limit was 0.003-16 μg/kg. CONCLUSIONS: The method is simple, stable and reproducible, and can be used for the determination of pesticide residues in M. alba.
期刊: 2016年第27卷第15期
作者: 黄莉莉,李丽莉,罗轶,陆敏仪,黄清泉
AUTHORS: HUANG Lili,LI Lili,LUO Yi,LU Minyi,HUANG Qingquan
关键字: 农药;桑叶;液相色谱-串联质谱法
KEYWORDS: Pesticide; Morus alba; LC-MS/MS
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