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,1.8μm)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5~1000μg/kg,检出限(S/N=3)为1.2μg/kg,甘蔗渣中线性范围为10~1000μg/kg,检出限(S/N=3)为2.7μg/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。
Objective 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,1.8μm),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 5-1000μg/kg,and the limits of detection(S/N=3)was 1.2μg/kg in sugarcane juice.The calibration range of 10-1000μg/kg and the limits of detection(S/N=3)was 2.7μg/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.
作者
胡重怡
李雨露
郭平
万建春
张威
王栋
HU Zhong-Yi;LI Yu-Lu;GUO Ping;WAN Jian-Chun;ZHANG Wei;WANG Dong(Jiangxi Institute for Food Control,Nanchang 330001,China)
出处
《食品安全质量检测学报》
CAS
2020年第2期521-527,共7页
Journal of Food Safety and Quality
基金
江西省科技厅重点研发项目(20192BBF60047)。
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
sugarcane
solid phase ultra-high performance liquid chromatography tandem mass spectrometry
3-nitropropionic acid
