摘要
建立了阴离子交换高效液相色谱-电感耦合等离子体质谱联用测定不同形态硒的在线分离检测方法,并将其应用于长期汞暴露人群血清中小分子硒的形态研究。流动相A为0.5 mmol/L柠檬酸铵-2%（V/V）甲醇（pH 3.7）,流动相B为100 mmol/L柠檬酸铵-2%（V/V）甲醇（pH 8.0）;采用93%A-7%B时,硒代半胱氨酸（SeCys）、硒代蛋氨酸（SeMet）、SeⅣ和SeⅣ的保留时间分别为2.48,3.28,5.19和7.02 min。采用基体匹配标准外标法定量,加标回收率为93%~117%;相对标准偏差小于9%;SeCys,SeMet,SeⅣ和SeⅣ的检出限分别为0.34,0.67,1.38和0.63 mg/L（S/N=3）。本方法已成功应用于研究长期汞暴露地区硒干预人群中血清中硒的化学形态研究。结果表明：血清中小分子硒主要是SeⅣ;补硒后,血清中总硒及SeⅣ含量均增加。
A hyphenated technique was optimized to simultaneously determine different selenium species,including SeⅣ,SeⅣ,selenocysteine（SeCys） and selenomethionine（SeMet）,by anion exchange（AE）-inductively coupled plasma mass spectrometry（ICP-MS）.Ammonium citrate and methanol were used as mobile phase.Mobile phase A is composed of 0.5 mmol/L ammonium citrate＋2%（V/V） methanol while mobile B is 100 mM ammonium citrate＋2%（V/V） methanol.When 93% A＋7% B were used,the four Se species can be separated in 7.5 min.The detection limits for SeCys,SeⅣ,SeMet and SeⅣ were 0.34,0.67,1.38 and 0.63 mg/L respectively,according to 3 times standard deviation of the blank criterion.The recoveries of spiked SeⅣ in serum samples were between 93% and 107% and the RSDs were less than 9%（n=3）.This method was applied to analyze serum samples from long-term mercury-exposed people supplemented with selenium-enriched yeast.The concentrations of total Se and SeⅣ in serum samples were found increased after Se supplementation.The method is simple,rapid,sensitive,repeatable,and suitable for speciation analysis of small molecular seleno-compounds in different biological samples.
出处
《分析化学》
SCIE
EI
CAS
CSCD
北大核心
2011年第4期466-470,共5页
Chinese Journal of Analytical Chemistry
基金
中国科学院重要方向性项目(No.KJCX3.CYW.N3)
国际原子能机构项目(NO.CPR-15818)
欧盟第六框架计划项目(No.FOOD-CT-2006-016253)
中国科学院高能物理研究所青年基金资助项目
关键词
阴离子交换色谱
电感耦合等离子体质谱
硒
形态
Anion exchange chromatography
Inductively coupled plasma mass spectrometry
Serum
Selenium species
