摘要
本研究建立EMR固相萃取结合超高效液相色谱-串联质谱测定虾肉中15种性激素残留的分析方法。样品采用0.1 mol/L乙二胺四乙酸二钠溶液-乙腈溶液提取,经Captiva EMR固相萃取SPE小柱净化,CAPCELLPAK C18 BB-H(3μm,2.1 mm×150 mm)色谱柱分离,电喷雾离子源正负离子分开扫描;多反应监测模式的超高效液相色谱-串联质联质谱法进行检测,以空白基质匹配外标法定量。正离子流动相为甲醇和0.1%甲酸,检测雄激素与孕激素;负离子流动相为乙腈和0.01%氨水溶液,检测雌激素。结果表明,经EMR固相萃取净化的虾肉样品中的15种性激素残留在1~50μg/kg浓度范围内线性关系良好,相关系数(r)均大于0.99,方法检出限为0.0015~0.436μg/kg,定量限为0.0051~1.453μg/kg,平均回收率在85.31%~119.84%,相对标准偏差为2.11%~9.86%(n=6)。本方法操作快速简单,重复性好,灵敏度较高,适用于虾肉中15种性激素残留的检测。
A method for the determination of 15 sex hormones in shrimp meat by EMR solid phase extraction combined with ultra performance liquid chromatography-tandem mass spectrometry was established. The samples was extracted with0.1 mol/L ethylenediaminetetraacetic acid disodium solution and acetonitrile solution, purified by Captiva EMR SPE cartridge, separated by CAPCELLPAK C18 BB-H(3 μm, 2.1 mm×150 mm) column, and scanned by positive and negative ions of electrospray ion source. Ultra performance liquid chromatography-tandem mass spectrometry(UPLC-MS/MS) with multiple reaction monitoring mode was used for detection, and blank matrix matching external standard method was used for quantification. The positive ion mobile phase was methanol and 0.1% formic acid, and androgen and progesterone were detected. The negative ion mobile phase was acetonitrile and 0.01% ammonia aqueous solution to detect estrogen. The results showed that the 15 kinds of sex hormone residues in shrimp meat samples purified by EMR solid phase extraction had a good linear relationship in the concentration range of 1~50 μg/kg, and the correlation coefficients(r) were all greater than 0.99. The detection limits of the method were 0.0015~0.436 μg/kg, and the quantitative limits were 0.0051~1.453 μg/kg.The average recoveries were 85.31%~119.84%, and the relative standard deviations were 2.11%~9.86%(n=6). The method was rapid, simple, reproducible and sensitive, which was suitable for the detection of 15 kinds of sex hormone residues in shrimp meat.
作者
辛丽娜
莫东淑
蒋定之
曾坚
梁飞燕
蒙初曦
XIN Lina;MO Dongshu;JIANG Dingzhi;ZENG Jian;LIANG Feiyan;MENG Chuxi(Guangxi-Asean Food and Drug Safety Inspection and Testing Center,Nanning 530021,China)
出处
《食品工业科技》
CAS
北大核心
2022年第2期263-270,共8页
Science and Technology of Food Industry
基金
广西-东盟食品检验检测中心科学研究项目(KY202103)。
关键词
超高效液相色谱-串联质谱法
EMR固相萃取柱
性激素
虾肉
雌二醇
炔雌醇
己烯雌酚
黄体酮
睾丸酮
ultra high performance liquid chromatography tandem mass spectrometry
captiva EMR-lipid
sex hormones
shrimp
estradiol
ethinylestradiol
diethylstilbestrol
progesterone
testosterone