多壁碳纳米管净化技术联合UPLC-MS/MS测定地表水中7种性激素残留  

Multi walled carbon nanotube purification technology combined with UPLC-MS/MS to determine seven residual sex hormones in surface water

作　　者：赵光骞 赵海军 李杰 ZHAO Guang-qian;ZHAO Hai-jun;LI Jie(Nanyang Ecological Environment Monitoring Center in Henan Province,Nanyang 473000,China;Ecological Environment Monitoring Emergency Center at the Head of the Middle Route of South to North Water Transfer in Henan Province,Nanyang 474475,China;Nanyang Sewage Purification Center,Nanyang 473000,China)

机构地区：[1]河南省南阳生态环境监测中心,河南南阳473000 [2]河南省南水北调中线渠首生态环境监测应急中心,河南南阳474475 [3]南阳市污水净化中心,河南南阳473000

出　　处：《化学研究与应用》2025年第3期572-578,共7页Chemical Research and Application

摘　　要：实验建立了多壁碳纳米管净化技术联合UPLC-MS/MS快速测定医药化工企业集聚区周边水塘中左炔诺孕酮、黄体酮、雌酮、甲基睾酮、雄烯二酮和甲羟孕酮含量的分析方法。随机采集医药化工企业集聚区周边水塘中地表水样品,去除异物,滤纸过滤,取预处理后的地表水样品500 mL,调节水样酸度至pH(7±0.05);精密吸取上述预处理后的水样25 mL,置50 mL具塞离心管中,加入10 mL乙腈、2.0 g乙酸钠和6.0 g无水硫酸镁,涡旋3 min,再以8000 r·min^(-1)的转速离心5 min;取上清液5.0 mL,置25 mL离心管中,加入20 mg多壁碳纳米管和300 mg无水硫酸镁,涡旋3 min使之充分混匀,再将离心管置高速冷冻离心机中以10000 r·min^(-1)速度离心5 min;取出离心管,上清液过滤,续滤液作为样品溶液,上UPLC-MS/MS仪定性、定量检测。左炔诺孕酮、黄体酮、雌酮、甲基睾酮、雄烯二酮和甲羟孕酮6种性激素在0.002~8.0 mg·L-1浓度范围内线性良好,相关系数(r)均大于0.995;检测限分别为0.005、0.004、0.009、0.006、0.008和0.003μg·L^(-1);三水平加标回收率均在81.3~92.3%之间。此方法具有准确、快速等优点,可以用于医药化工企业集聚区周边水塘中左炔诺孕酮、黄体酮、雌酮、甲基睾酮、雄烯二酮和甲羟孕酮等常见性激素的监测。An analytical method for rapid determination of levonorgestrel,progesterone,estrone,methyltestosterone,androstendione and medroxyprogesterone in the surrounding water pool of pharmaceutical and chemical enterprises was established by using multiwall carbon nanotube purification technology combined with UPLC-MS/MS.Surface water samples were randomly collected from ponds around the gathering area of pharmaceutical and chemical enterprises.Samples were removed foreign bodies and filtered with filter paper.500 mL of pre-treated surface water samples were taken and adjusted the acidity of the water samples to pH(7±0.05).25 mL of the pre-treated water sample was precisely absorbed into a 50 mL plugged centrifuge tube,10 mL acetonitrile,2.0 g sodium acetate and 6.0 g anhydrous magnesium sulfate were added,vortex for 3 min,and then centrifuge at a rotating speed of 8000 r·min^(-1)for 5 min.5.0 mL of supernatant were taken and placed in 25 mL centrifuge tube,20 mg multi-wall carbon nanotubes and 300mg anhydrous magnesium sulfate were added,swirled it for 3 min to thoroughly mix,and then centrifuged the centrifuge in a highspeed refrigerated centrifuge at a speed of 10000 r·min^(-1)for 5 min.The centrifugal tube was removed,the supernatant was filtered,and the further filtrate was used as the sample solution,and UPLC-MS/MS instrument was used for qualitative and quantitative detection.Levonorgestrel,progesterone,estrone,methyltestosterone,androstendione and medroxyprogesterone showed good linear relationships in the concentration ranges of 0.002~8.0 mg·L^(-1),with correlation coefficients(r)all greater than 0.995;Detection limits were 0.005、0.004、0.009、0.006、0.008 and 0.003μg·L^(-1),respectively.Average recoveries in 3 concentration levels were 81.3~92.3%.This method has the advantages of accuracy and speed,and can be used for the monitoring of levonorgestrel,progesterone,estrone,methyl testosterone,androstendione and medroxyprogesterone in the surrounding water pool of pharmaceutical and chemical enterprises

关 键 词：多壁碳纳米管 UPLC-MS/MS 医药化工 周边水塘 左炔诺孕酮 

分 类 号：O657.7[理学—分析化学]