高效液相色谱-电喷雾串联质谱法测定婴幼儿奶粉中对羟基苯甲酸酯类防腐剂
Determination of parabens in infant milk powders by high performance liquid chromatography-electrospray ionization tandem mass spectrometry
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摘要: 建立了高效液相色谱-串联质谱法检测奶粉中8种对羟基苯甲酸酯类防腐剂的分析方法.样品以乙腈为提取溶剂,经HLB固相萃取柱富集净化,分别用甲醇和丙酮溶液洗脱,洗脱液经氮吹浓缩定容后,高效液相色谱-串联质谱仪进行分析.8种对羟基苯甲酸酯加标浓度在5、50、100 ng·g-1时的回收率分别为71.1%—96.1%、72.8%—99.8%和78.8%—118%,相对标准偏差(RSD)为3.2%—10%(n=5),内标法定量,方法检出限为0.04—0.43 ng·g-1.将建立的方法应用于市场常见品牌的婴幼儿奶粉样品的分析,结果表明7个品牌奶粉样品中共有5种防腐剂检出.
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关键词:
- 高效液相色谱-串联质谱 /
- 对羟基苯甲酸酯 /
- 防腐剂 /
- 婴幼儿奶粉
Abstract: A method for the determination of 8 parabens in infant milk powders by using high performance liquid chromatography-electrospray ionization tandem mass spectrometry was developed. The target preservatives in infant milk powders were extracted by acetonitrile and cleaned-up by HLB solid-phrase extraction, and then eluted with methanol and acetone solutions respectively. The eluate was collected and concentrated under a gentle stream of nitrogen gas, and then analyzed by HPLC-ESI-MS/MS. The recoveries of 8 parabens in infant milk powders at 3 levels (5,10 and 100 ng·g-1) were 78.8%-118%,72.8%-99.8% and 71.1%-96.1% and relative standard deviation (RSD, n=5) was 3.2%-10%. The method detection limits were 0.04-0.43 ng·g-1. This developed method was applied to analyze the infant milk powders in Beijing and results showed that some PBs were detected all in seven samples. -
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