干旱区生态环境知识资源中心(Arid): 超高效液相色谱-串联质谱法同时测定奶粉中8种雌激素残留

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	超高效液相色谱-串联质谱法同时测定奶粉中8种雌激素残留
其他题名	Determination of 8 estrogen residues in milk powder by UPLC-MS/MS
	赵超群; 李樱红; 刘柱; 罗金文
来源期刊	药物分析杂志
ISSN	0254-1793
出版年	2020
卷号	40 期号:2
中文摘要	目的:建立超高效液相色谱-串联质谱法(UPLC-MS/MS法)同时测定奶粉中8种雌激素残留。方法:0.5 g奶粉样品用2.0 mL温水溶解,经8.0 mL 0.1%甲酸-乙腈提取,通过离心去除沉淀后,将上清液过Waters oasis Prime-HLB(6 CC,200 mg)柱净化,收集洗脱液于40 ℃氮吹至近干,复溶后采用Waters CORTECS T_3(2.1 mm*50 mm,2.7 mum)色谱柱,以0.1%氨水溶液和乙腈为流动相进行梯度洗脱。在电喷雾离子源负离子(ESI-)模式下电离,以多反应监测模式(MRM)进行质谱检测。结果:8种激素残留在定量下限到20倍定量下限范围内有良好的线性关系,相关系数(R~2)均大于0.99,检测下限(LOD)为0.33~2.07 mug·kg~(-1),定量下限(LOQ)为0.98~6.21 mug·kg~(-1),3种加标水平下平均回收率在95.2%~118.1%之间,RSD(n=6)均小于6.7%。采用已建立的方法,对10批市售奶粉样品进行检测,结果样品中均含有内源性雌激素,检出beta-雌二醇、alpha-雌二醇、雌酮。结论:实验所建立方法简便,灵敏,实用性强,可同时测定牛奶中的8种雌激素残留,适用于日常监测工作。
英文摘要	Objective:To establish a method for the simultaneous determination of 8 estrogen residues in milk powder by UPLC-MS/MS.Methods:0.5 g milk powder sample was dissolved in 2.0 mL warm water,the target compounds was extracted by 8.0 mL 0.1% formic acid-acetonitrile,the precipitate was removed by centrifugation,and the clear supernatant extract was purified by Waters oasis Prime-HLB(6 CC,200 mg).The separation and analysis were performed on a Waters CORTECS T_3(2.1 mm*50 mm,2.7 mum).The mobile phase consisted of 0.1% ammonia aqueous solution and acetonitrile with gradient elution.Ionization was conducted under the negative ion(ESI-) mode of the electrospray ion source,and mass spectrometry was detected by multiple reaction monitoring mode(MRM).Results:Good linear relationships were obtained between the quantitative limits and 20-fold quantitative limits of 8 estrogens.The correlation coefficients(R~2) were greater than 0.99,the limit of detection (LOD) was 0.33-2.07 mug·kg~(-1),the limit of quantitative(LOQ) was 0.98-6.21 mug·kg~(-1),the average recoveries were 95.2%-118.1% at the three levels,and the relative standard deviations(n=6) below 6.7%.The established method was used to test 10 batches of marketable milk power.The results showed that all the samples contained 17-beta-estadiol,17-alpha-estradiol and estrone.Conclusion:The established method is simple,sensitive and practical,and suitable for the simultaneous determination of 8 estrogen residues in milk power.
中文关键词	超高效液相色谱-串联质谱法 ; 固相萃取 ; 奶粉 ; 雌激素残留 ; 定性定量分析
英文关键词	UPLC-MS/MS solid phase extraction milk powder estrogen residues qualitative and quantitative analysis
类型	Article
语种	中文
收录类别	CSCD
WOS类目	Pharmacology & Pharmacy
CSCD记录号	CSCD:6729353
资源类型	期刊论文
条目标识符	http://119.78.100.177/qdio/handle/2XILL650/353960
作者单位	赵超群, 浙江省食品药品检验研究院, 杭州, 浙江 310052, 中国. 李樱红, 浙江省食品药品检验研究院, 杭州, 浙江 310052, 中国. 刘柱, 浙江省食品药品检验研究院, 杭州, 浙江 310052, 中国. 罗金文, 浙江省食品药品检验研究院, 杭州, 浙江 310052, 中国.
推荐引用方式 GB/T 7714	赵超群,李樱红,刘柱,等. 超高效液相色谱-串联质谱法同时测定奶粉中8种雌激素残留[J],2020,40(2).
APA	赵超群,李樱红,刘柱,&罗金文.(2020).超高效液相色谱-串联质谱法同时测定奶粉中8种雌激素残留.药物分析杂志,40(2).
MLA	赵超群,et al."超高效液相色谱-串联质谱法同时测定奶粉中8种雌激素残留".药物分析杂志 40.2(2020).