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作 者:张宁 汪文龙 李韵晴 王新航 司露露 唐深[3] 陆彩玲 秦富 李习艺[1] ZHANG Ning;WANG Wenlong;LI Yunqing;WANG Xinhang;SI Lulu;TANG Shen;LU Cailing;QIN Fu;LI Xiyi(School of Public Health,Guangxi Medical University,Nanning 530021;Customs Technology Center of Nanning,Nanning 530021;School of Preclinical Medicine,Guangxi Medical University,Nanning 530021)
机构地区:[1]广西医科大学公共卫生学院,广西南宁530021 [2]南宁海关技术中心,广西南宁530021 [3]广西医科大学基础医学院,广西南宁530021
出 处:《分析科学学报》2020年第6期879-883,共5页Journal of Analytical Science
基 金:国家自然科学基金(No.81860585);广西自然科学基金(No.2018GXNSFAA281130)。
摘 要:建立了同时检测大鼠肝脏中S-腺苷甲硫氨酸(SAM)和S-腺苷同型半胱氨酸(SAH)的高效液相色谱-串联质谱法。肝脏样品匀浆后用5.0 mmol/L NH4Ac+0.4%HAc+2%甲醇提取,采用CORTES UPLC-C18+柱分离,在电喷雾电离正离子模式(ESI+)下,以多反应监测(MRM)检测,外标法定量。SAM在0.1~2.0μg/mL范围内线性关系良好(R2=0.997);SAH在0.01~0.20μg/mL范围内线性关系良好(R2=0.999);SAM和SAH的方法定量限(S/N>10)分别为0.250、0.025μg/g;幼年SD大鼠肝脏中SAM和SAH的含量分别为86.34±5.54μg/g、17.73±2.24μg/g;相对标准偏差分别是6.4%和11.5%。该方法灵敏度高、特异性强,适用于大鼠肝脏组织中SAM和SAH的同时测定。A fast confirmation method for determination of S-adenosylmethionine(SAM) and S-adenosylhomocysteine(SAH) in rat liver by high performance liquid chromatography-tandem mass spectrometry(HPLC-MS/MS) was established.The samples were extracted with an aqueous solution containing 5 mmol/L ammonium acetate,0.4% acetic acid and 2% methanol.The compounds were tested by positive electrospray ion source(ESI^+) and multiple reaction monitoring(MRM) mode.The correlation coefficients(R^2) were greater than 0.997,which indicated that the linear dependence of SAM and SAH were good in the range of 0.1-2.0 μg/mL and 0.01-0.2 μg/mL.The limits of quantitation(S/N>10) of SAM and SAH were 0.250 μg/g and 0.025 μg/g,respectively.The contents of SAM and SAH in the liver of SD rats were 86.34±5.54 μg/g and 17.73±2.24 μg/g,and the relative standard deviations(RSDs,n=6) of SAM and SAH were 6.4% and 11.5%,respectively.The method is featured with good accuracy and high sensitivity,and has been successfully applied to the detection of SAM and SAH in rat liver.
关 键 词:高效液相色谱-串联质谱 S-腺苷甲硫氨酸 S-腺苷同型半胱氨酸 大鼠肝脏
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