摘要
建立了同时测定水产品中辛酚、4-壬基酚、双酚、己烯雌酚、雌酮、17β-雌二醇、17α-乙炔雌二醇和雌三醇的超高效液相色谱串联质谱法。样品经乙酸乙酯提取2次，HLB固相萃取柱净化，提取液氮吹至干，残渣用甲醇-水（体积比1：9）溶解。以甲醇和5mmol乙酸铵-0．1％甲酸溶液为流动相，经ACQU—ITY^TM BEHC18色谱柱分离后进行LC—MS／MS多反应监测模式的定性及定量分析，外标法定量。方法检出限为0．1～0．3μg/kg。在添加水平为0．3～5．0μg/kg范围内的平均回收率为81％～108％，相对标准偏差为6．7％～11．4％。该方法灵敏度高、操作简单高效，适用于水产品中8种雌激素的定量及确证分析。
An ultra performance liquid chromatography- electrospray ionization triple-quadruple tan- dem mass spectrometric（UPLC -ESI MS/MS） method has been established for the simultaneous determination of 8 estrogens, including octylphenol, 4-nonylphenol, bishphenol A, diethylstilbestrol, estrone, 17/3-estradiol, 17α-ethinylestradiol and estriol, in aquatic products. The estrogens were extracted twice by ethyl acetate and cleaned up on a HLB solid phase extraction column. The extract was evaporated to dryness under nitrogen, and redissolved in methanol - water（ 1 ： 9, by volume）. The separation of 8 estrogens was carried out by a ACQUITYTM BEH Cls column（ 100 mm× 2. 1 mm i. d. , 1.7 μm） using methanol（A） and 5 mmol/L ammonium acetate -0. 1% formic acid（B） as the mobile phases. The target compounds were confirmed and quantified by MS - MS under multiplereaction monitoring （MRM） mode with external standard method. Extraction and chromatographic conditions were optimized and the best separation was obtained. Under the optimal conditions, the limits of detection（LODs） ranged from 0. 1 μg/kg to 0. 3 μg/kg, and the average recoveries of 8 estrogens at spiked concentration of 0.3 -5.0 μg/kg were in the range of 81% -108%. The relative standard deviations（RSDs） ranged from 6.7% to 11.4%. The method was effective, simple and sensitive, and was suitable for the determination and confirmation of estrogens in aquatic products.
出处
《分析测试学报》
CAS
CSCD
北大核心
2010年第2期152-156,共5页
Journal of Instrumental Analysis
基金
山东省科技攻关资助项目(2008GG10005005)
海洋公益性行业科研专项经费资助项目(200805031)
山东省水生动物营养与饲料泰山学者岗位资助项目
关键词
超高效液相色谱质谱法
水产品
雌激素
ultra performance liquid chromatography - electrospray ionization triple-quadruple tan- dem mass spectrometry（UPLC -ESI MS/MS）
aquatic products
estrogens
