黄油中8种类固醇激素的液相色谱/串联质谱检测

建立了黄油中雌酮、α-雌二醇、β-雌二醇、雌三醇、睾酮、表睾酮、孕酮和丙酸睾酮8种类固醇激素的凝胶渗透色谱（GPC）-液相色谱/串联质谱（LC-MS/MS）检测方法.样品用乙酸乙酯-环己烷（1∶1,V/V）提取,提取液经GPC柱净化除脂,GPC浓缩液采用C18色谱柱（100 mm±215;2.0 mm i.d.,3.0μm）分离,以乙腈和水为流动相进行梯度洗脱,电喷雾电离多反应监测模式进行定性和定量分析.8种类固醇激素以基质匹配外标法定量,药物在1.0～20.0 μg/kg线性范围内相关系数（r）均大于0.999;方法检出限（S/N=3）为0.04 ～0.30μg/kg,定量限LOQs（S/N...

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Published in分析化学 Vol. 42; no. 3; pp. 360 - 366
Main Author 赵超敏 岳振峰 吴晖 欧阳姗 赖富饶 肖陈贵 张毅 康海宁 华红慧
Format Journal Article
LanguageChinese
Published 华南理工大学轻工与食品学院,广州,510640%深圳出入境检验检疫局食品检验检疫技术中心,深圳市食品安全检测技术研发重点实验室,深圳518045%中山大学生命科学学院,广州,510275 2014
Subjects
凝胶渗透色谱
孕激素
液相色谱-串联质谱
雄性激素
雌性激素
黄油
孕激素
Androgens
Progestin
黄油
液相色谱-串联质谱
Estrogens
Butter
雌性激素
Liquid chromatography-tandem mass spectrometry
雄性激素
凝胶渗透色谱
Gel permeation chromatography
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ISSN0253-3820
DOI10.3724/SP.J.1096.2014.30857

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Summary:建立了黄油中雌酮、α-雌二醇、β-雌二醇、雌三醇、睾酮、表睾酮、孕酮和丙酸睾酮8种类固醇激素的凝胶渗透色谱（GPC）-液相色谱/串联质谱（LC-MS/MS）检测方法.样品用乙酸乙酯-环己烷（1∶1,V/V）提取,提取液经GPC柱净化除脂,GPC浓缩液采用C18色谱柱（100 mm±215;2.0 mm i.d.,3.0μm）分离,以乙腈和水为流动相进行梯度洗脱,电喷雾电离多反应监测模式进行定性和定量分析.8种类固醇激素以基质匹配外标法定量,药物在1.0～20.0 μg/kg线性范围内相关系数（r）均大于0.999;方法检出限（S/N=3）为0.04 ～0.30μg/kg,定量限LOQs（S/N=10）为1.0 μg/kg;添加水平为1.0,2.0,4.0 μg/ks时,回收率范围在64.1％～110％之间;相对标准偏差（RSD）小于11％.结果表明,本方法准确、可靠,满足黄油中8种类固醇激素的检测分析要求.
Bibliography:A method was developed for the determination of eight steroid hormones （estrone, α/β-estradiol, estriol, testosterone, epitestosterone, progesterone and testosterone propionate） in butter samples by gel permeation chromatography （GPC） purification-followed by liquid chromatography-tandem mass spectrometry （LC-MS/MS）. The samples were first extracted by ethylacetate/cyclohexane （ 1： 1, V/V） and the extract was later degreased by GPC column. Then, the GPC concentrate was separated using a C18 column （ 100 mm x 2.0 mm i. d. , 3.0 μm） with gradient elution of acetonitrile/water. Finally, the steroid hormone components were qualitatively and quantitatively determined by mass spectrometer with electrospray ionization in multi reaction monitoring mode. Using matrix matched external standard method, good linearity in response could be obtained in the concentration range of 1.0-20.0 μg/kg with correlation co-efficiency larger than 0. 999. The detection limits of the method were 0.04-0.30 p,g/kg and the quantification
ISSN:0253-3820
DOI:10.3724/SP.J.1096.2014.30857