超高效液相色谱法测定食品中的多种防腐剂

Simultaneous determination of multiple preservatives in food using ultra performance liquid chromatography

目的:建立了超高效液相色谱(UPLC)法测定食品中14种防腐剂的定性定量分析方法。方法:样品用饱和氯化钠、乙腈、正己烷3种溶液萃取提取,正己烷提取溶液经凝胶渗透色谱(GPC)净化后与乙腈提取溶液合并注入超高效液相色谱分析。14种化合物经ACQUITY UPLCTMBEH C18柱(150 mm×2.1 mm,1.7μm)柱分离,以乙酸铵-乙腈溶液作为流动相进行梯度洗脱,紫外检测器(UV)检测,检测波长为280 nm。结果:14种化合物在线性范围内具有较好的线性关系,相关系数(r)>0.99,定量限(LOQ)在0.01 mg/kg～0.6 mg/kg之间;空白样品添加回收率在63.4%～99.5%之间,精密度(RSD)在0.490%～16.3%之间。结论:该方法适用于食品中防腐剂的检测。

Objective： An ultra performance liquid chromatography （UPLC） method was developed for the simultaneous deter- mination of 14 preservatives in food. Methods： The samples were extracted using liquidliquid extraction with saturated NaCl, acetonitrile and hexane. The extract in hexane was purified using GPC, and then combined with the extract in aeetonitrile, finally, the mixed liquid was analyzed by UPLC. The analytes were separated on ACQUITY UPLCTM BEH ClS column using aeetonitrile - ammonium acetate as mobile phase for gradient elution, then detected under UV detector with detection wavelength of 280 nm. Re- sults： The correlation coefficient of this method had good linearity （ r 〉 0.99 ） , the limits of quantification （ LOQs ） ranged from 0.01 mg/kg to 0.6 mg/kg. The recoveries at spiked levels ranged from 63.4% to 99.5%, the relative standard deviations （RSD） ranged from 0.490% to 16.3%. Conclusion： The method can be applied for the determination of preservatives in food.