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

作　　者：于瀛[1,2] 张晶[2] 刘洪涛[1] 邵兵[2] 

机构地区：[1]北京化工大学理学院,应用化学北京100029 [2]北京市疾病预防控制中心,北京100013

出　　处：《中国食品卫生杂志》2009年第6期489-493,共5页Chinese Journal of Food Hygiene

基　　金：北京市科委资助项目(D08050200310802)

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。Objective A new ultra performance liquid chromatography/tandem mass spectrometry （UPLC-MS/MS） method was developed to analyze natamyein 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 C18 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 muhi-reaetion 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 ttg/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 eoncentration 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 eould be applied to the identification and quantification of natamycin residues in jam.

关 键 词：色谱法 高压液相 光谱法 质量 电喷雾电离 纳他霉素 果酱 

分 类 号：R155.5[医药卫生—营养与食品卫生学]