Determination of Four Aflatoxins in Shanyao Pills by UPLC-MS/MS
Objective To establish an ultra-high performance liquid chromatography-mass spectrometry(UPLC-MS/MS)method for simultaneous determination of four aflatoxins in Shanyao Pills.Methods The sample was extracted with 70％methanol and purified by the QuEChERS purification tubes and immunoaffinity columns.The chromatographic column was Acquity UPLC BEH C18 column(100 mm × 2.1 mm,1.7 μm),the mobile phase was acetonitrile-10 mmol/L ammonium acetate solution(gradient elution),the flow rate was 0.20 mL/min,the column temperature was 25 ℃,and the injection volume was 2 μL.Multi-reaction monitoring mode was adopted with electric spray ion and positive ion scanning,the capillary voltage was 2.4 kV,the desolvation gas temperature was 450 ℃,and the flow rate was 950 L/h.Results The linear ranges of aflatoxins B1,B2,G1,and G2 were 0.108-2.160 ng/mL,0.033-0.660 ng/mL,0.101-2.020 ng/mL,and 0.030-0.600 ng/mL(r ≥ 0.998,n=5),respectively.The RSDs of precision,stability,and repeatability tests were all lower than 4.0％(n=6).The average recoveries of aflatoxins B1,B2,G1,and G2 were 93.00％,87.22％,87.88％,and 87.44％,with RSDs of 1.63％,3.05％,1.85％,and 3.26％(n=6),respectively.Six batches of samples were detected with aflatoxin contents of 0.6,0.5,1.4,0.9,0.9,and 0.8 μg/kg,respectively.Conclusion The method is simple,highly sensitive,fast,accurate,and highly specific,which can be used for the simultaneously determination of four aflatoxins in Shanyao Pills.
万方数据
维普
