摘要
建立了婴配乳粉中炔诺酮、21α-羟基孕酮、17α-羟基孕酮、甲基炔诺酮、甲羟孕酮、乙酸甲地孕酮、乙酸氯地孕酮、甲羟孕酮乙酸酯、孕酮的UPLC-MS/MS检测方法。样品经溶解、沉淀蛋白后提取孕激素,通过除脂、净化、浓缩等步骤获得样液,采用超高效液相色谱分离、三重四极杆质谱仪进行检测,内标定量。通过优化前处理条件, 9种孕激素(炔诺酮线性范围2.5~100 ng/mL,其余线性范围1~40 ng/mL)线性关系良好, R2均大于0.995;方法定量限为0.4~1.0μg/kg,相对标准偏差(n=10)为0.71%~10.95%,炔诺酮在加标量为1, 2和10μg/kg时回收率为77.4%~102.5%,其他8种在加标量为0.4, 0.8和4μg/kg时回收率为62.2%~112.6%。该方法能对婴配乳粉中9种孕激素同时测定,操作简单,具有良好的准确性、灵敏性、特异性,可为婴配乳粉风险监控方法提供参考。
Establish an analytical method for the determination of 9 kinds of progestational hormone residues including norethisterone,21a-hydroxyprogesterone,17a-hydroxyprogesterone,norgestrel,medroxyprogesterone,megestrol acetate,chlormadinone acetate,medroxyprogesterone acetate,and progesterone by ultra high performance liquid chromatography tandem triple quadrupole mass spectrometry.The infant formula milk powder was dissolved in water,the protein was precipitated with organic reagent,then the progestational hormone residue was extracted.After that,the final sample solution was obtained through the steps of fat removal,purification and concentration.The solution was separated by ultra-high performance liquid chromatography,detected by triple quadrupole mass spectrometer,and quantitatively analyzed by internal standard.By optimizing the pretreatment conditions,9 kinds of progestational hormone had good linear relationship(the range of norethisterone was 2.5-100 ng/mL,and the others were 1-40 ng/mL),and the determination coeficient R'>0.995.The SLoo for these 9 compounds ranged from 0.4μg/kg to 1.0μg/kg,and the Srsd(n=10)ranged from 0.71%to 10.95%.The spike recoveries were 62.2%-112.6%(norethisterone recovery was 77.4%-102.5%in spiking 1,2 and 10μg/kg,and the others were 62.2%-112.6%in spiking 0.4,0.8 and 4μg/kg).The method could simultaneously determine 9 kinds of progestational hormone in infant formula milk powder.It was simple,accurate,sensitive and specific,and could provide a reference for the risk monitoring method of infant formula milk powder.
作者
葛城
张浩
刘钢
詹胜群
周荣杰
GE Cheng;ZHANG Hao;LIU Gang;ZHAN Shengqun;ZHOU Rongjie(Ausnutria Dairy(China)Co,Ltd.,Changsha 410200)
出处
《食品工业》
CAS
2023年第3期317-322,共6页
The Food Industry
