摘要
目的建立超高效液相色谱-串联质谱法测定硒代蛋氨酸(SeMet)的方法,并用于测定牛奶中游离SeMet。方法在Acquity UPLC BEH C18。色谱柱(2.1mm×100mm,1.7um)上以水:乙腈:甲酸(95:5:0.1, V/V)为流动相,流速0.3mL/min,柱温40℃,分析时间2.5min,在电喷雾一正离子电离源上以多反应监测模式分析SeMet,用于定量分析的离子反应为m/z198.0—181.1。结果SeMet线性范围为0.5~100ng/mL,方法的定量下限为0.5ng/mL。SeMet批内准确度在97.6%~100.6%,批间准确度在97.7%~99.2%,批内精密度在0.53%~4.49%,批间精密度在1.03%~4.54%。结论UPLC.MS/MS法具有特异性好、灵敏度高、分析速度快和准确可靠的优点,适用于牛奶中游离SeMet的定量测定。
Objective To establish an ultra-performance liquid chromatography-tandem mass spectrometry (UPLC-MS/MS) method for the quantification of free selenomethionine (SeMet), and be applied to the quantification of free SeMet in cow milk. Methods The analyte was separated on a BEH C18 column (2. 1 mm x 100 mm, 1.7 μm) at 40 ℃ with a mobile phase of water: acetonitrile: formic acid(95: 5: 0. 1, V/V) , a flow rate of 0. 3 mL/ min, and an analysis time of 2. 5 min. At positive electrospray ionization mode, multiple reaction monitoring of the precursor-product ion transitions of m/z 198.0-181.1 was used for the quantification. Results The linear calibration curve was obtained in a concentration range of 0.5 - 100 ng/mL with a lower limit of quantification of 0. 5 ng/mL. The value of intra- and inter-day accuracy for SeMet fell in the range of 97.6%-100. 6% and 97.7%- 99. 2% , and value of intra- and inter-day precision 0. 53%- 4. 49% and 1.03%- 4. 54%. Conclusion The method is specific, sensitive, rapid, and accurate, suitable for the quantification of free SeMet in cow milk.
出处
《卫生研究》
CAS
CSCD
北大核心
2016年第1期65-67,97,共4页
Journal of Hygiene Research
基金
国家自然科学基金(No.81372989)
中国营养学会营养科研基金-伊利营养与健康研究基金(No.2013-013)