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超高效液相色谱-质谱法测定果酱中纳他霉素残留
Determination of Natamycin in Jam by Ultra Performance Liquid Chromatography with Tandem Mass Spectrometry
【摘要】 目的建立了果酱中纳他霉素的超高效液相色谱-串联质谱(UPLC-MS/MS)检测方法。方法样品加入0.5g氯化钠、经10ml丙酮萃取,以甲醇-水溶液为流动相进行梯度洗脱,经BEHC18色谱柱分离,通过多反应监测模式(MRM)进行测定。结果纳他霉素在蓝莓果酱、葡萄树莓果酱、香蕉草莓果酱、黄桃果酱、苹果果酱和山楂草莓果酱中的线性范围分别为0.5~25.0、0.5~25.0、1.0~25.0、1.0~25.0、0.5~25.0和1.0~25.0μg/kg,相关系数(R2)均大于0.99。6种果酱中目标化合物的定量限为0.5~1.0μg/kg,3个浓度水平的加标回收率为80.1%~113.3%,相对标准偏差(RSD,n=5)小于20%。结论该方法快速、准确、操作简便,可用于果酱中纳他霉素的确证和定量分析。
【Abstract】 Objective A new ultra performance liquid chromatography/tandem mass spectrometry(UPLC-MS/MS)method was developed to analyze natamycin in jam.Method After adding 0.5 g NaCl,2 g of jam samples were extracted by 10 ml acetone and separated on a BEH C_ 18 column using a binary mobile phase of methanol and water.As a result,well-shaped peak can be obtained on the chromatogram of analyte under the multi-reaction monitoring(MRM)mode.Results The assay for natamycin in jams of blueberry,grape raspberry,banana strawberry,peach,apple and hawthorn strawberry were linear over the range of 0.5-25.0,0.5-25.0,1.0-25.0,1.0-25.0,0.5-25.0,and 1.0-25.0 μg/kg respectively,with correlation coefficient(R2)>0.99.Limits of quantification(LOQ)in these jam samples ranged from 0.5 to 1.0 μg/kg,and the recovery(spiked in each jam at three concentration levels)ranged of 80.1%-113.3%,with relative standard deviations(RSD,n=5)less than 20%.Conclusion UPLC-MS/MS method is a rapid,simple and highly sensitive method,which could be applied to the identification and quantification of natamycin residues in jam.
【Key words】 Chromatography,Liquid; Spectrometry,Mass,Electrospray Ionization; Natamycin; Jam;
- 【文献出处】 中国食品卫生杂志 ,Chinese Journal of Food Hygiene , 编辑部邮箱 ,2009年06期
- 【分类号】R155.5
- 【被引频次】5
- 【下载频次】248