采用快速溶剂萃取-高效液相色谱-电感耦合等离子体质谱法（HPLC-ICP-MS）快速测定淀粉类农作物中硒酸根、亚硒酸根、甲基-硒代半胱氨酸和硒代蛋氨酸4种形态硒的含量。称取经冷冻干燥粉碎的样品0.300 0 g，加入0.03 g蛋白酶XIV，以水为提取剂，于40 ℃下快速萃取25 min。所得提取液用水定容至100.0 mL后立即用超滤离心管过滤，滤液采用Hypersil Gold C₈色谱柱进行分离，以20 mmol·L^-1磷酸二氢钾-0.1%（体积分数）七氟丁酸-5%（体积分数）甲醇混合溶液为流动相进行等度洗脱，采用电感耦合等离子体质谱法测定洗脱液中4种形态硒的含量。4种硒形态在6 min内可实现有效的色谱分离，质量浓度在一定范围内与其峰面积呈线性关系，方法检出限（3.14s）为0.05~0.10 mg·kg^-1。样品加标回收率为81.6%~110%，测定值的相对标准偏差（n=6）为2.1%~11%。

A method was established for rapid simultaneous determination of 4 species of selenium[including selenate, selenite, (Methyl) seleno-cysteine and selenomethionine] in starchy crops using accelerated solvent extraction (ASE) combined with HPLC-ICP-MS. The freeze-dried and crushed samples (0.300 0 g) was added into 0.03 g of protease XIV, and the mixture was rapidly extracted at 40℃ for 25 min with water as extraction agent. The extract was made up to 100.0 mL with water, and filtered by ultrafiltration centrifuge tube immediately. The 4 species of selenium were separated on a Hypersil Gold C₈ chromatographic column, with using 20 mmol·L^-1 potassium dihydrogen phosphate-0.1% (volume fraction) heptafluorobutyric acid-5% (volume fraction) methanol as mobile phase for isocratic elution. ICP-MS was used to determine the 4 species of selenium in the eluate. The results showed that the 4 selenium species were separated effectively in 6 min. Linear relationships between peak area and mass concentration of the 4 selenium species were kept in the definite range. Limits of detection were found in the range of 0.05-0.10 mg·kg^-1. Values of recovery obtained by standard addition method were in the range of 81.6%-110%, and RSDs (n=6) were in the range of 2.1%-11%.