1. 浙江工业大学化学工程与材料学院
2. 浙江省质量检测科学研究院
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张晓波, 黄丽英, 陈小珍, 等. UFLC-IT-TOF-MS分析婴幼儿配方乳粉中的12种雌孕激素[J]. 分析测试学报, 2013,32(11):1289-1295.
Determination of 12 Kinds of Estrogenic and Progesterone Hormones in Infant Formula Milk Powder by Ultra Fast Liquid Chromatography-Ion Trap-Time of Flight Mass Spectrometry[J]. 2013,32(11):1289-1295.
建立了婴幼儿配方乳粉中12种雌孕激素的超快速液相色谱-离子阱-飞行时间串联质谱(UFLC-IT-TOF-MS)测定方法。乳粉样品在37 ℃水溶解、酶解后,经乙腈提取,HLB柱净化,Shim-pack XR-ODSⅡ和HSS T3色谱柱梯度分离,采用电喷雾离子源(ESI)负离子模式对雌激素进行分析,正离子模式对孕激素进行分析。12种雌孕激素在1.0~200 μg/L 范围内线性关系均良好(r2>0.998),平均回收率为79.9%~110.4%,相对标准偏差为2.8%~8.0%,检出限和定量下限分别为0.3~0.6 μg/kg及0.9~1.8 μg/kg。实验考察了12种雌孕激素精确质量数的测定能力并验证了雌酮的三级裂解。
A method was developed for the determination of 12 kinds of estrogenic and progesterone hormones in infant formula milk powder using ultra fast liquid chromatography-ion trap-time of flight mass spectrometry(UFLC-IT-TOF-MS).The milk powder was dissolved in warm water,and extracted with ethyl acetate after enzymatic hydrolysis.The extract was cleaned up on an HLB cartridge.The estrogenic and progesterone hormones were separated on Shim pack XR-ODSⅡand HSS T3 columns,and then analyzed in ESI- mode for estrogens and ESI+ mode for progesterones.The calibration curves of the target compounds were linear in the range of 1.0-200 μg/L with correlation coefficients greater than 0.998.The average spiked recoveries were in the range of 79.9%-110.4% with relative standard deviations of 2.8%-8.0%.The limits of detection(LODs) ranged from 0.3 μg/kg to 0.6 μg/kg and the limits of quantitation(LOQ) ranged from 0.9 μg/kg to 1.8 μg/kg.The mass errors between theoretical and experimental masses were obtained for deprotonated molecule of 12 estrogenic and progesterone hormones,and the main possible fragmentation pathway of estrone was verified.
液相色谱-离子阱-飞行时间串联质谱雌孕激素婴幼儿配方乳粉
ultra fast liquid chromatography-ion trap-time of flight mass spectrometry(UFLC-IT-TOF-MS)estrogenic and progesterone hormonesinfant formula milk powder
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