高效液相色谱-质谱联用法测定薏苡仁药材中黄曲霉毒素

Determination of aflatoxin in coix seed by high performance liquid chromatography-mass spectrometry

中文关键词:  高效液相色谱-质谱联用法  黄曲霉毒素  薏苡仁

英文关键词:high performance liquid chromatography-mass spectrometry  aflatoxins  coix seed

中文摘要:

      目的 建立高效液相色谱-质谱联用法(high performance liquid chromatography-mass spectrometer, HPLC-MS)测定薏苡仁中药饮片中黄曲霉毒素B1、B2、G1、G2的方法, 并对比不同产地薏苡仁中黄曲霉毒素含量。方法 样品经过免疫亲合柱处理后, 采用HPLC-MS进行测定。分析柱为C18柱(50 mm×2.1 mm, 1.8 μm), 流动相为10 mmol/L醋酸铵溶液-甲醇溶液, 梯度洗脱, 流速为0.3 mL/min, 柱温为25 ℃。结果 黄曲霉毒素B1在0.26~10.4 ng/mL浓度范围内与峰面积值均呈现良好的线性关系(r2=0.9995), 平均加样回收率为75.4%~123.9%, 黄曲霉毒素B2在0.0875~3.5 ng/mL浓度范围内与峰面积值均呈现良好的线性关系(r2=0.9996), 平均加样回收率为71.1%~124.2%, 黄曲霉毒素G1在0.295~11.89 ng/mL浓度范围内与峰面积值均呈现良好的线性关系(r2=0.9995), 平均加样回收率为78.9%~112.2%, 黄曲霉毒素G2在0.1475~5.9 ng/mL浓度范围内与峰面积值均呈现良好的线性关系(r2=0.9992), 平均加样回收率为73.8%~123.9%。结论 该方法准确、可靠、专属性强, 通过精确化合物离子监测, 可准确的测定薏苡仁中黄曲霉毒素含量。

英文摘要:

      Objective To establish a method for the determination of aflatoxin B1, B2, G1 and G2 in coix seed by high performance liquid chromatography-mass spectrometry (UPLC-MS), and compare the aflatoxin content in coix seed from different producing areas. Methods The samples were treated by immune affinity column, and detected by UPLC-MS. Analysis column was C18 column (50 mm×2.1 mm, 1.8 μm), the mobile phase was gradient elution with 10 mmol/L ammonium acetate solution-methanol, flow rate was 0.3 mL/min, and column temperature was 25 ℃. Results Aflatoxin B1 had good linear relationships in the range of 0.26-10.4 ng/mL, and the correlation coefficient was 0.9995. The average recoveries of aflatoxin B1 were 75.4%-123.9%. Aflatoxin B2 had good linear relationships in the range of 0.0875-3.5 ng/mL, and the correlation coefficient was 0.9996. The average recoveries of aflatoxin B2 were 71.1%-124.2%. Aflatoxin G1 had good linear relationships in the range of 0.295-11.89 ng/mL, and the correlation coefficient was 0.9995. The average recoveries of aflatoxin G1 were 78.9%~112.2%. Aflatoxin G2 had good linear relationships in the range of 0.1475-5.9 ng/mL ng/mL, and the correlation coefficient was 0.9992. The average recoveries of aflatoxin G2 were 73.8%-123.9%. Conclusion This method is accurate, reliable and specific, and can accurately determine the aflatoxin content in coix seed by precise compound ion monitoring.