论文部分内容阅读
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。
An anion-exchange high performance liquid chromatography-inductively coupled plasma mass spectrometry (ICP-MS / MS / MS) method was developed for the on-line separation and determination of different forms of selenium and applied to the study on the morphology of small molecules of selenium in human serum exposed to long-term mercury exposure. The mobile phase A was 0.5 mmol / L ammonium citrate 2% (V / V) methanol (pH 3.7) and the mobile phase B was 100 mmol / L ammonium citrate 2% (V / V) The retention times of selenocysteine (SeCys), SeMet, SeⅣ and SeⅣ with 93% A-7% B were 2.48, 3.28, 5.19 and 7.02 min, respectively. The detection limits of SeCys, SeMet, SeⅣ and Se Ⅳ were 0.34, 0.67, 1.38 and 0.63 mg / L, respectively. The detection limits of SeCys, SeMet, SeⅣ and SeⅣ were 93% ~ 117% and the relative standard deviations were less than 9% (S / N = 3). The method has been successfully applied to study the chemical forms of selenium in the selenium intervention population exposed to long-term mercury exposure. The results showed that the main selenium in serum was SeⅣ. After selenium supplementation, the contents of total selenium and Se Ⅳ in serum increased.