干旱区生态环境知识资源中心(Arid): 奶粉中高氯酸盐的液相色谱-串联质谱测定

Arid

	奶粉中高氯酸盐的液相色谱-串联质谱测定
其他题名	Determination of Perchlorate in Milk Powder Using Liquid Chromatography-Mass Spectrometry
	黄晓兰; 罗辉泰; 吴惠勤; 朱志鑫; 黄芳; 林晓珊
ISSN	1004-4957
出版年	2009
卷号	28 期号:8 页码:896-899,904
中文摘要	建立了奶粉中高氯酸盐的液相色谱-串联质谱(LC-MS/MS)测定方法.奶粉样品用水-乙腈(体积比1:2)超声波振荡提取2次,于4 000 r/min离心后,上清液经Oasis HLB固相萃取小柱净化;采用离子交换色谱分离,色谱柱为METROSEP A Supp 5(150 mm*4.0 mm)阴离子交换柱,流动相为0.2 mol/L乙酸铵溶液-乙腈(体积比1 : 1),流速0.7 mL/min;电喷雾负离子模式电离,质谱多反应选择离子检测(MRM),检测离子对为 m/z 9983和m/z 10185,其中m/z 9983为定量离子对.方法的相对标准偏差为3.59%,回收率为91% ～106%,检出限为1.0 mug/kg,定量下限为5.0 mug/kg.结果表明,该法简便快速、准确可靠,也适用于鲜牛奶、酸牛奶等其他乳制品中高氯酸盐的测定.
英文摘要	A liquid chromatography-mass spectrometry(LC-MS/MS) method was developed for determination of perchlorate in milk powder.Perchlorate in milk powder was extracted twice by sonication with water and acetonitrile(1∶2,by volume).The extract was centrifugalized at 4 000 r/min,and cleaned up on Oasis HLB solid phase extraction(SPE) column.The separation of perchlorate was performed on an anion ion exchange column METROSEP A Supp 5(150 mm*4.0 mm) using acetonitrile-0.2 mol/L ammonium acetate(1∶1,by volume) as the mobile phase with flow rate of 0.7 mL/min.The analysis of perchlorate was carried out under negative ESI MS/MS and multiple-reaction monitoring mode(MRM) by selecting m/z 9983 and m/z 10185 as qualitative ions,and m/z 9983 as quantitative ion.The extraction conditions and experimental parameters were also optimized.Under the optimal conditions,the calibration curve showed a good linearity over perchlorate concentration in the range of 6.2-620 mug/L.The spiked recoveries of perchlorate were in the range of 91%-106% with RSD of 3.59%.The detection limit and quantitation limit were 1.0 mug/kg and 5.0 mug/kg,respectively.The method was proved to be simple and accurate,and was suitable for the determination of perchlorate in milk powder and other dairy products such as fresh milk,sour milk,etc.
中文关键词	高氯酸盐 ; 液相色谱-串联质谱 ; 奶粉 ; 乳制品
英文关键词	perchlorate liquid chromatography -mass spectrometry(LC - MS/MS) milk powder dairy product
语种	中文
国家	中国
收录类别	CSCD
WOS类目	CHEMISTRY ANALYTICAL ; ENGINEERING CHEMICAL
WOS研究方向	Chemistry ; Engineering
CSCD记录号	CSCD:3656807
资源类型	期刊论文
条目标识符	http://119.78.100.177/qdio/handle/2XILL650/223483
作者单位	中国广州分析测试中心, 广东省化学危害应急检测技术重点实验室, 广州, 广东 510070, 中国
推荐引用方式 GB/T 7714	黄晓兰,罗辉泰,吴惠勤,等. 奶粉中高氯酸盐的液相色谱-串联质谱测定[J],2009,28(8):896-899,904.
APA	黄晓兰,罗辉泰,吴惠勤,朱志鑫,黄芳,&林晓珊.(2009).奶粉中高氯酸盐的液相色谱-串联质谱测定.,28(8),896-899,904.
MLA	黄晓兰,et al."奶粉中高氯酸盐的液相色谱-串联质谱测定".28.8(2009):896-899,904.