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：5μl;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0.003~16μg/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。
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 was69.3%-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.
出处
《中国药房》
CAS
北大核心
2016年第15期2122-2126,共5页
China Pharmacy
