摘要
采用高效液相色谱-质谱联用(HPLC-MS)技术,在负离子扫描模式下建立了原料奶的乙腈提取成分的指纹图谱。采用乙腈和0.1%的乙酸水溶液为流动相进行二元梯度洗脱,柱温30℃,分析时间为85min。确定了11个共有峰,以其中的7号峰为参照物,通过相对峰面积和相对保留时间进行了方法学考察。结果表明,本方法具有良好的重现性,各指纹峰相对保留时间的相对标准偏差(RSD)小于0.79%,相对峰面积的RSD小于2.84%。在原料奶指纹图谱基础上,选取有代表性的危害物如防腐剂苯甲酸等进行了添加,建立了危害物添加图谱,对沈阳地区超市的50个纯牛奶样品进行了筛查,取得初步的应用结果。
The fingerprint of raw milk based on high performance liquid chromatography-mass spectrometry （HPLC-MS） in negative ion mode was established to evaluate the quality of raw milk. The raw milk was extracted by acetonitrile and the obtained constituents were eluted by acetonitrile and 0.1% acetic acid solution with a gradient program at a column temperature of 30 ℃ within 85 min. A total of 11 common peaks had been identified. The methodology was investigated by the relative peak area and relative retention time with No. 7 peak as the reference. The results showed that the fingerprint established by this method has reasonable reproducibility with the relative standard deviations （RSDs） less than 0.79% for the relative retention time and less than 2.84% for the relative peak area. Based on the fingerprint,a labelling HPLC-MS spectrogram was obtained for the screening of hazards by adding several representative hazards,such as benzoic acid etc. An amount of 50 pure milk samples in Shenyang supermarkets were inspected,and preliminary results had been achieved.
出处
《色谱》
CAS
CSCD
北大核心
2010年第10期935-939,共5页
Chinese Journal of Chromatography
基金
中国科学院重要方向项目(No.KSCX2-YW-N-035)
沈阳市重大科技支撑计划项目(No.1071110-9-01)
关键词
高效液相色谱-质谱联用
指纹图谱
原料奶
high performance liquid chromatography-mass spectrometry （HPLC-MS）
fingerprint
raw milk
