谷类食品中硒形态超声酶提取-高效液相色谱-电感耦合等离子体质谱法测定

陈绍占; 唐德剑; 李晓玉; 夏曾润; 刘丽萍

doi:10.11847/zgggws1122301

谷类食品中硒形态超声酶提取-高效液相色谱-电感耦合等离子体质谱法测定

Determination of selenium species in cereal food with ultrasonic enzyme extraction and high performance liquid chromatography-inductively coupled plasma mass spectrometry

摘要

摘要:
目的采用高效液相色谱 – 电感耦合等离子体质谱法研究谷类食品中的硒形态。
方法采用Hamilton PRP-X100阴离子交换柱作为分析柱，40 mmol/L磷酸氢二铵（NH₄）₂HPO₄（pH = 5.0）和60 mmol/L（NH₄）₂HPO₄（pH = 6.0）为流动相，梯度洗脱，硒代胱氨酸（SeCys₂）、甲基硒代半胱氨酸（MeSeCys）、亚硒酸盐Se（IV）、硒代蛋氨酸（SeMet）和硒酸盐Se（VI）可在16 min内实现基线分离。采用超声辅助酶提取法对谷类食品进行预处理。
结果 SeCys₂、MeSeCys、Se（IV）、SeMet和Se（VI）的方法检出限分别为2.5、5.0、2.5、10.0和5.0 μg/kg；0.5～200.0 μg/L范围内，线性相关系数（r）均 > 0.999，线性关系良好。
结论谷类食品中的硒形态主要以硒代蛋氨酸为主，同时含有少量硒代胱氨酸、无机硒及一些未知的硒化合物。

Abstract:
Objective To detect selenium species in cereal food using high performance liquid chromatography-inductively coupled plasma mass spectrometry (HPLC-ICP-MS).
Methods Hamilton PRP-X100 anion exchange column was used as analytical column; 40 mmol/L diammonium phosphate (pH = 5.0) and 60 mmol/L diammonium phosphate (pH = 6.0) were used as mobile phase for gradient elution. Baseline separation of selenocysteine (SeCys₂), methylselenocysteine (MeSeCys), selenite Se(IV), selenomethionine (SeMet), and selenate Se(VI) were completed in 16 minutes. Ultrasonic-assisted enzyme extraction was used to extract selenium species in cereal food samples.
Results The method detection limit for SeCys₂, MeSeCys, Se(IV), SeMet, and Se(VI) were 2.5, 5.0, 2.5, 10.0, and 5.0 μg/kg, respectively. The linear correlation coefficients (r) were all greater than 0.999 in the range of 0.5 – 200.0 μg/L for the detections.
Conclusion Selenomethionine is a main selenium species, with a small amount of selenocystine, inorganic selenium and some unknown selenium compounds being detected, in cereal food.

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