Determination of Residues of Steroid Hormone Drugs and Related Drug in Surface Water Around Medical and Chemical Park by Ultra-High Performance Liquid Chromatography-Tandem Mass Spectrometry with Automatic Solid Phase Extraction
摘 要
以全自动固相萃取-超高效液相色谱-串联质谱法测定医化园区周边地表水中地塞米松、泼尼松、炔诺酮、炔雌醇、甲睾酮和米非司酮的残留量。随机采集医化园区周边地表水样,除杂后置于棕色广口瓶中,将其酸度调至pH 7。分取500 mL水样,以10 mL·min-1流量过活化好的HLB固相萃取柱,用20%(体积分数)甲醇溶液15 mL洗脱,收集洗脱液,于50℃氮吹至近干,残渣用甲醇复溶并定容至1 mL,涡旋30 s,按照优化的仪器工作条件测定。以Agilent Zorbax Eclipse Plus C18色谱柱为固定相,以不同体积比的1 mmol·L-1乙酸铵溶液和乙腈的混合溶液为流动相进行梯度洗脱,分离所得目标物用三重四极杆串联质谱仪在电喷雾离子源负离子模式以及多反应监测模式下检测,外标法定量。结果显示,6种目标物的质量浓度均在0.005~5 mg·L-1内与其对应的峰面积呈线性关系,检出限(3S/N)分别为0.24,0.14,0.51,0.16,0.21,0.08 μg·L-1;对实际样品进行3个浓度水平的加标回收试验,6种目标化合物的回收率为83.9%~105%,测定值的相对标准偏差(n=5)为2.7%~4.1%,在样品中检出了地塞米松和炔雌醇,检出量分别为0.75,1.27 μg·L-1。
Abstract
Residues of dexamethasone, prednisone, norethindrone, ethinylestradiol, methyltestosterone and mifepristone in surface water around medical and chemical park by ultra-high performance liquid chromatography-tandem mass spectrometry with automatic solid phase extraction (SPE). Surface water sample around medical and chemical park was randomly collected, and impurities in which were removed. The solution obtained was placed in a brown jar, and its acidity was adjust to pH 7. An aliquot (500 mL) of the water sample was passed through HLB SPE column activated beforehand at flow rate of 10 mL·min-1, and the column was eluted with 15 mL of 20% (volume fraction) methanol solution. The eluate was collected and blown to nearly dry by nitrogen at 50 ℃, and the residue was redissolved and diluted to 1 mL with methanol. After mixing by vortex for 30 s, the mixed solution was analyzed by the optimized instrument working conditions. Agilent Zorbax Eclipse Plus C18 column was used as the stationary phase, and the mixed solutions composed of 1 mmol·L-1 ammonium acetate solution and acetonitrile at different volume ratios were used as mobile phase for gradient elution. The separated targets were detected by triple quadrupole tandem mass spectrometer in electrospray ion source negative ion mode and multiple reaction monitoring mode, and quantified by external standard method. It was shown that linear relationships between values of the peak area and the mass concentration of the 6 targets were kept in the same range of 0.005-5 mg·L-1, with detection limits (3S/N) of 0.24, 0.14, 0.51, 0.16, 0.21, 0.08 μg·L-1, respectively. Test for the spiked recovery was made on actual samples at the 3 concentration levels, giving recoveries of the 6 targets in the range of 83.9%-105%, with RSDs (n=5) of the determined values ranged from 2.7% to 4.1%, and dexamethasone and ethinylestradiol were detected at 0.75, 1.27 μg·L-1 in the sample, respectively.
中图分类号 O657.63 DOI 10.11973/lhjy-hx202208012
所属栏目 工作简报
基金项目
收稿日期 2021/1/26
修改稿日期
网络出版日期
作者单位点击查看
备注李旭霞,高级工程师,主要从事环境监测工作,934086166@qq.com
引用该论文: LI Xuxia. Determination of Residues of Steroid Hormone Drugs and Related Drug in Surface Water Around Medical and Chemical Park by Ultra-High Performance Liquid Chromatography-Tandem Mass Spectrometry with Automatic Solid Phase Extraction[J]. Physical Testing and Chemical Analysis part B:Chemical Analysis, 2022, 58(8): 939~943
李旭霞. 全自动固相萃取-超高效液相色谱-串联质谱法测定医化园区周边地表水中甾体激素类及相关药物的残留量[J]. 理化检验-化学分册, 2022, 58(8): 939~943
共有人对该论文发表了看法,其中:
人认为该论文很差
人认为该论文较差
人认为该论文一般
人认为该论文较好
人认为该论文很好
参考文献
【1】谭俊波,罗元政,张志彬.中印两国纺织品产业内贸易影响因素分析[J].武汉纺织大学学报, 2018,31(3):3-9.
【2】王晖,丁苗,饶钦全,等.典型医化园区废气和环境空气中挥发性有机物污染特征[J].环境监控与预警, 2018,10(6):43-47.
【3】李泽建,饶思原.电子商务产业园生态系统结构与运行机制研究-基于共生理论视角[J].科技和产业, 2020,20(5):8-14.
【4】白陈仲,魏东斌,杜宇国,等.环境水体中9种内分泌干扰物的同时高效富集方法[J].环境化学, 2016,35(4):680-687.
【5】司秀荣,徐东耀.环境内分泌干扰物前处理方法研究新进展[J].环境科学与管理, 2011,36(8):60-64.
【6】吴根义,廖新俤,贺德春,等.我国畜禽养殖污染防治现状及对策[J].农业环境科学学报, 2014,33(7):1261-1264.
【7】葛璇,刘莉,王明泉,等.固相萃取-液相色谱-串联质谱法测定水中5种雌激素[J].中国环境监测, 2014,30(5):73-76.
【8】李佩佩,郭远明,陈雪昌,等.凝胶渗透色谱-固相萃取/高效液相色谱法同时测定水产品中甲基睾酮与己烯雌酚[J].分析测试学报, 2013,32(2):267-270.
【9】朱娟.研究甾体激素类药物治疗女性生殖内分泌疾病的效果与安全性[J].中外医学研究, 2019,17(18):137-139.
【10】刘玉萍,邹跃琼,马霞,等.女性生殖内分泌疾病应用甾体激素的疗效观察[J].实用妇科内分泌电子杂志, 2015,2(6):155-156.
【11】吴杰群,徐顺清,王鸿,等.生物转化甾醇制备甾体药物中间体研究进展[J].中国医药工业杂志, 2020,51(7):801-814.
【12】刘夺,张莹,周晓,等.合成生物技术生产甾体激素中间体的研究展望[J].生命科学, 2013,25(10):958-965.
【13】刘萌萌.地塞米松加炉甘石洗剂治疗过敏性皮炎的效果评估[J].首都食品与医药, 2019,26(4):56-56.
【14】周新明.泼尼松联合茶碱治疗中老年人支气管哮喘的效果研究[J].数理医药学杂志, 2020,33(7):1038-1039.
【15】樊逸雯,王素霞,陈进康.多囊卵巢综合征患者使用激素避孕的非避孕益处和挑战[J].中国乡村医药, 2020,27(7):77-78.
【16】杨金泉,贺小敏,施敏芳,等.固相萃取-超高效液相色谱-串联质谱法同时测定地表水中9种性激素[J].中国环境监测, 2019,35(3):19-27.
【2】王晖,丁苗,饶钦全,等.典型医化园区废气和环境空气中挥发性有机物污染特征[J].环境监控与预警, 2018,10(6):43-47.
【3】李泽建,饶思原.电子商务产业园生态系统结构与运行机制研究-基于共生理论视角[J].科技和产业, 2020,20(5):8-14.
【4】白陈仲,魏东斌,杜宇国,等.环境水体中9种内分泌干扰物的同时高效富集方法[J].环境化学, 2016,35(4):680-687.
【5】司秀荣,徐东耀.环境内分泌干扰物前处理方法研究新进展[J].环境科学与管理, 2011,36(8):60-64.
【6】吴根义,廖新俤,贺德春,等.我国畜禽养殖污染防治现状及对策[J].农业环境科学学报, 2014,33(7):1261-1264.
【7】葛璇,刘莉,王明泉,等.固相萃取-液相色谱-串联质谱法测定水中5种雌激素[J].中国环境监测, 2014,30(5):73-76.
【8】李佩佩,郭远明,陈雪昌,等.凝胶渗透色谱-固相萃取/高效液相色谱法同时测定水产品中甲基睾酮与己烯雌酚[J].分析测试学报, 2013,32(2):267-270.
【9】朱娟.研究甾体激素类药物治疗女性生殖内分泌疾病的效果与安全性[J].中外医学研究, 2019,17(18):137-139.
【10】刘玉萍,邹跃琼,马霞,等.女性生殖内分泌疾病应用甾体激素的疗效观察[J].实用妇科内分泌电子杂志, 2015,2(6):155-156.
【11】吴杰群,徐顺清,王鸿,等.生物转化甾醇制备甾体药物中间体研究进展[J].中国医药工业杂志, 2020,51(7):801-814.
【12】刘夺,张莹,周晓,等.合成生物技术生产甾体激素中间体的研究展望[J].生命科学, 2013,25(10):958-965.
【13】刘萌萌.地塞米松加炉甘石洗剂治疗过敏性皮炎的效果评估[J].首都食品与医药, 2019,26(4):56-56.
【14】周新明.泼尼松联合茶碱治疗中老年人支气管哮喘的效果研究[J].数理医药学杂志, 2020,33(7):1038-1039.
【15】樊逸雯,王素霞,陈进康.多囊卵巢综合征患者使用激素避孕的非避孕益处和挑战[J].中国乡村医药, 2020,27(7):77-78.
【16】杨金泉,贺小敏,施敏芳,等.固相萃取-超高效液相色谱-串联质谱法同时测定地表水中9种性激素[J].中国环境监测, 2019,35(3):19-27.
相关信息