L-硒-甲基硒代半胱氨酸是一种新型硒源类的食品营养强化剂，而D-硒-甲基硒代半胱氨酸的安全性尚没有相关研究，目前对于L-硒-甲基硒代半胱氨酸含量的测定方法多集中在测定硒-甲基硒代半胱氨酸含量，无法检测到其中L-硒-甲基硒代半胱氨酸的含量。本文建立了通过手性色谱柱分离、标准曲线法测定L-硒-甲基硒代半胱氨酸的高效液相色谱法(HPLC)。实验使用EC250/4 NUCLEOSIL Chiral-1手性色谱柱(4 mm×250 mm，5 μm)，流动相为0.4mmol/L CuSO4?5H2O水溶液，柱温为35 ℃，流速为1.0 mL/min，进样量为20 μL，检测波长为240 nm；在该条件下 L-硒-甲基硒代半胱氨酸的检测线性范围为0.541~1.352 mg/ml，线性相关系数R达0.9999，在线性范围内精密度和稳定性良好，平均回收率为97.73%。该方法操作简单，结果准确，可用于L-硒-甲基硒代半胱氨酸产品及其制品质量的监控。

L-Se-methylselenocysteine is a new selenium-containing food supplement; however, no studies regarding the safety of D-Se-methylselenocysteine have been reported. Current methods for the determination of L-Se-methylselenocysteine content mainly focus on the measurement of total Se-methylselenocysteine content and cannot differentiate it from the content of L-Se-methylselenocysteine. High-pressure liquid chromatography (HPLC) was used in this study to estimate L-Se-methylselenocysteine content using chiral separation, and a standard curve was established. Reliable chromatographic separation was achieved on an EC250/4 NUCLEOSIL Chiral-1 column (4 mm × 250 mm, 5 μm) when the mobile phase was 0.4 mmol/L CuSO4?5H2O, column temperature was 35 ℃, flow rate was 1.0 mL/min, sample size was 20 μL, and detection wavelength was 240 nm. Under these conditions, the calibration curves established showed good linearity across the concentration range of 0.541~1.352 mg/ml, with a correlation coefficient of 0.9999 and an average recovery of 97.73%. The method is simple, accurate, and can be used to monitor the quality of L-Se-methylselenocysteine and its related products.

食品安全国家标准制定项目(spaq-2013-30)；江西省博士后科研项目（2013KY04）