摘要
目的建立甘蔗中3-硝基丙酸的固相萃取-超高效液相色谱串联质谱检测方法。方法样品经乙腈萃取,Sep-pak氨基固相萃取柱净化,超高效液相色谱串联质谱法测定甘蔗中3-硝基丙酸含量。色谱柱为WatersACQUITY BEH C18柱(1.7μm,50 mm×2.1 mm),柱温40℃,样品温度10℃,进样体积5μl,流动相A为水,流动相B为乙腈,梯度洗脱。结果方法的线性范围为4.0～40.0μg/kg,基质加标工作曲线线性相关系数为0.998。方法的定性检出限为1.0μg/kg,定量检出限为4.0μg/kg。高、中、低3个浓度水平的加标回收率为92.5%～93.6%,相对标准偏差小于10%。结论本方法灵敏、快速、准确,可用于甘蔗中3-硝基丙酸的测定。
Objective To establish a method for the detection of 3-nitropropionic acid in sugarcane by solid-phase extraction（SPE） coupled with ultra high performance liquid chromatography-tandem mass spectrometry（UPLC-MS/MS）.Methods Samples were extracted by acetonitrile and cleaned up by Sep-pak NH2 solid phase extraction column.The 3-nitropropionic acid was determined by UPLC-MS/MS.The chromatographic conditions： using Waters ACQUITY BEH C18 column（1.7 μm,50 mm×2.1 mm） with water as mobile phase A and acetonitrile as mobile phase B for gradient elution;keeping the column temperature at 40 ℃ and the samples at 10 ℃ with an injection volume of 5 μl.Results There was a good linearity of the calibration curve for 3-nitropropionic acid standard in the range of 4.0-40.0 μg/kg with correlation coefficient of 0.998.The detection limit of the method was 1.0 μg/kg and the limit of quantification was 4.0 μg/kg.The average recovery at three spiked levels was in the range of 92.5%-93.6%,and the relative standard derivation was lower than 10%.Conclusion The method is simple,rapid,sensitive and accurate,which can be used in the detection of 3-nitropropionic acid in sugar cane.
出处
《中国食品卫生杂志》
北大核心
2012年第2期127-132,共6页
Chinese Journal of Food Hygiene
