固相萃取-超高效液相色谱-三重四极杆质谱法测定甘蔗中3-硝基丙酸

Determination of 3-nitropropionic acid in sugarcane by solid phase ultra performance liquid chromatography tandem mass spectrometry

中文关键词:  甘蔗  固相萃取-超高效液相色谱-三重四极杆质谱法  3-硝基丙酸

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

中文摘要:

      目的 建立固相萃取-超高效液相色谱-三重四极杆质谱联用技术(solid phase extraction-ultra performance liquid chromatography tandem mass spectrometry, SPE-UPLC-MS/MS)测定甘蔗中3-硝基丙酸(3-nitropropionic acid, 3-NPA)的分析方法。方法 甘蔗汁和甘蔗渣经PSA固相萃取提取净化, 以1%氨水甲醇溶液洗脱, 氮吹吹干定容于0.5%甲酸水溶液中, 以Waters HSS T3色谱柱(2.1 mm×50 mm, 1.8 μm)在流动相乙腈-水(1:1, V:V)条件下进行分离, 电喷雾负离子MRM模式下检测, 以基质标准曲线定量。结果 甘蔗汁中3-硝基丙酸的线性范围为5~1000 μg/kg, 检出限(S/N=3)为1.2 μg/kg, 甘蔗渣中线性范围为10~1000 μg/kg, 检出限(S/N=3)为2.7 μg/kg。甘蔗汁和甘蔗渣3-NPA的加标回收率为96.5%~101.2%, 相对标准偏差为1.54%~5.35%。结论 该方法简单、灵敏、准确, 可用于甘蔗中3-硝基丙酸检测。

英文摘要:

      To establish a method for the determination of 3-nitropropionic acid (3-NPA) in sugarcane by solid phase extraction-ultra performance liquid chromatography tandem mass spectrometry(SPE-UPLC-MS/MS). Methods 3-NPA was extracted and purified by PSA-SPE in sugarcane juice and sugarcane slag, eluted with 1% ammonia methanol solution, nitrogen blowed to dry, and finally dissolved in 0.5% formic acid aqueous solution. Chromatographic separation was performed on Waters HSS T3 column (2.1 mm×50 mm, 1.8 μm), using a mobile phase of (1:1, V:V) acetonitrile aqueous solution for separation. 3-NPA was detected by using negative electrospray ionization tandem mass spectrometry in multiple reaction monitoring (MRM) mode and quantitated via matrix standard curve. Results The linear range of 3-nitropropionic acid in sugarcane juice was 5?1000 μg/kg, and the limits of detection (S/N=3) was 1.2 μg/kg in sugarcane juice. The calibration range of 10?1000 μg/kg and the limits of detection (S/N=3) was 2.7 μg/kg in sugarcane slag. The recovery rate of 3-NPA in sugarcane juice and sugarcane slag was between 96.5%?101.2%, and the relative standard deviation was between 1.54%?5.35%. Conclusion This method is simple, sensitive and accurate, and can be used to detect 3-NPA in sugarcane.