论文部分内容阅读
目的建立聚酰胺(Polyamide,简称PA)小柱净化超快速液相色谱-电喷雾串联四极杆质谱(UFLC-MS/MS)测定食品中非法添加物酸性橙Ⅱ的方法。方法样品经甲醇-乙酸铵溶液振荡提取后用PA SPE柱净化,以乙腈-乙酸铵缓冲溶液为流动相,在C18色谱柱上经梯度洗脱分离后以多反应监测质谱测定(m/z 327.0→170.0,327.0→156.0)。结果方法的最低定量浓度为0.015 mg/kg,回收率为94%~96%之间,校准曲线的线性相关系数为0.9990,线性范围为0.4μg/ml~4.0μg/ml,并用于实际样品分析。结论该方法快速、准确、灵敏,能够满足食品中非法添加物酸性橙Ⅱ的测定要求。
OBJECTIVE To establish a method for the determination of acidic orange II in food by Polyamide (PA) column supercritical liquid chromatography-electrospray ionization tandem mass spectrometry (UFLC-MS / MS). Methods The samples were extracted by methanol-ammonium acetate solution, purified by PA SPE column, eluted with acetonitrile-ammonium acetate buffer solution by gradient elution on C18 column and detected by multiple reaction monitoring mass spectrometry (m / z 327.0 → 170.0, 327.0 → 156.0). Results The minimum concentration of the method was 0.015 mg / kg and the recoveries were between 94% and 96%. The calibration curve had a linear correlation coefficient of 0.9990 with a linear range of 0.4μg / ml ~ 4.0μg / ml and was used for the real sample analysis . Conclusion The method is rapid, accurate and sensitive and can meet the determination requirements of acid orange Ⅱ, an illegal additive in food.