环境固体样品中多种甾体激素的同步检测方法及条件优化  

Development and Optimization of an Analysis Method for Simultaneously Detecting Multiple Steroid Hormones in Environmental Solid Samples

作　　者：冯慧 徐欣 彭鹏 王馨凝 钟琴 邹华[1,3] 张云 FENG Hui;XU Xin;PENG Peng;WANG Xinning;ZHONG Qin;ZOU Hua;ZHANG Yun(School of Environmental and Civil Engineering,Jiangnan University,Wuxi 214122,China;Dongzhu Ecological Environment Protection Co.,Ltd.,Wuxi 214101,China;Jiangsu Collaborative Innovation Center of Technology and Material of Water Treatment,Suzhou University of Science and Technology,Suzhou 215009,China)

机构地区：[1]江南大学环境与土木工程学院,江苏无锡214122 [2]东珠生态环保股份有限公司,江苏无锡214101 [3]苏州科技大学,江苏省水处理技术与材料协同创新中心,江苏苏州215009

出　　处：《中国环境监测》2023年第2期214-224,共11页Environmental Monitoring in China

基　　金：国家自然科学基金青年基金项目(41807489);中国博士后科学基金项目(2021M691273);江苏省博士后科研资助计划项目(2021K482C);江苏省研究生科研与实践创新计划项目(KYCX201950);江苏省高等学校大学生创新创业训练计划项目(202110295158Y);江苏省“双创博士(世界名校类)”(1126010241180640)。

摘　　要：采用超声辅助萃取-吸附剂净化-液相色谱-串联质谱同步检测环境固体样品中22种甾体激素,比较筛选了超声辅助萃取的有机溶剂和净化萃取液的吸附剂。结果表明,使用甲醇/乙腈/乙腈对固体样品中的甾体激素分别进行3次超声辅助萃取效果最佳,在0~150 mg/mL投加量范围内,N-丙基乙二胺粉末能有效减少浓缩萃取液中有机质的干扰并获得最高回收率,石墨碳粉末的有机质去除效果最好,但同时也造成目标物的显著损失,而硅胶粉末对有机质的去除效果不明显,因此选用N-丙基乙二胺粉末为萃取液的净化吸附剂,推荐使用量为150~400 mg/mL,在此优化条件下,22种甾体激素的标准曲线线性良好,方法检出限为0.025~0.696μg/kg,加标回收率达到63.5%以上,且操作简便、耗时短,适用于各种复杂环境固体样品的检测分析。By comparing the performance of organic extraction solvents and cleanup adsorbents,a method combining ultrasonic-assisted extraction,adsorptive cleanup,and liquid chromatography-tandem mass spectrometry was optimized and used for simultaneous determination of 22 steroids in complex solid samples.The results showed that the best solvent combination for thrice sequential ultrasonic-assisted extraction was methanol,acetonitrile,and acetonitrile.Within the range of 0-150 mg/mL,primary secondary amine powder could effectively reduce the interference of organic matter in the concentrated extract and obtain the highest recoveries;ENVI Carb~(TM) powder showed the best removal of organic matter,but also caused significant loss of the target steroids;silica gel powder did not show obvious removal of organic matter.As a result,primary secondary amine was selected for the cleanup of the steroid extract,and the recommended dosage range was 150-400 mg/mL.Under the optimized conditions,the method showed good performance with standard curves of good linearity,low method detection limits of 0.025-0.696 μg/kg,and good recoveries above 63.5%.This method is simple,time-saving,and applicable for simultaneous determination of 22 steroids in various complex environmental solid samples.

关 键 词：甾体激素 超声辅助萃取 萃取液净化 固体样品 有机质干扰 

分 类 号：X830[环境科学与工程—环境工程]