高效液相色谱-串联质谱法测定甘蔗中的3-硝基丙酸含量

Determination of 3-nitropropionic acid in sugarcane by high liquid chromatography-tandem mass spectrometry

中文关键词:  3-硝基丙酸  固相萃取  高效液相色谱-串联质谱法

英文关键词:3-nitropropionic acid  solid phase extraction  high performance liquid chromatography-tandem mass spectrometry

中文摘要:

      目的 建立高效液相色谱-串联质谱法(high liquid chromatography-tandem mass spectrometry, HPLC- MS/MS)检测甘蔗中的3-硝基丙酸含量。方法 样品经乙腈提取, 经Sep-pak氨基柱固相萃取净化, 再经Merck seQuantTM Zic-Hilic(150 mm×2.1 mm, 5 μm)色谱柱分离, 以10 mmol/L甲酸铵-0.1%甲酸和乙腈为流动相进行梯度洗脱, 采用电喷雾负离子(electrospray ionization, ESI-)模式进行HPLC-MS/MS测定。结果 3-硝基丙酸在0.005~0.1 mg/L浓度范围内呈良好的线性关系, 工作曲线的回归方程为Y=4.48X+46.72, 相关系数为0.9994, 该方法的检出限为0.0036 mg/kg, 定量限为0.0119 mg/kg。在0.02、0.08和0.1 mg/kg加标水平下, 3-硝基丙酸的平均回收率为80.0%~96.8%, 相对标准偏差为1.90%~8.69%(n=6)。结论 本方法快捷、灵敏度高、结果准确, 可适用于甘蔗中的3-硝基丙酸的检测。

英文摘要:

      Objective To establish a method for the determination of 3-nitropropionic acid (3-NPA) in sugarcane by high performance liquid chromatography-tandem mass spectrometry (HPLC-MS/MS). Methods Samples were extracted with acetonitrile, cleaned by solid phase extraction column of Sep-pakan NH2, separated by the column of Merck seQuantTM Zic-Hilic (150 mm×2.1 mm, 5 μm) with 10 mmol/L ammonium formate-0.1% formic acid and acetonitrile as mobile phase for gradient elution, and detected by HPLC-MS/MS with the mode of electrospray ionization (ESI-). Results 3-NPA had a good linear relationship in the range of 0.005~0.1 mg/L with the correlation coefficient of 0.9994, and the regression equation was Y=4.48X+46.72. The limit of detection was 0.0036 mg/kg, and the limit of quantification was 0.0119 mg/kg. The average recoveries spiked at 3 levels of 0.02, 0.08 and 0.1 mg/kg were 80.0%~96.8% with relative standard deviations of 1.90%~8.69% (n=6). Conclusion The established method is rapid, sensitive and accurate, which is suitable for the determination of 3-nitropropionic acid in sugarcane.