同位素稀释气相色谱-质谱法快速测定酱油中3-氯-1,2-丙二醇量

采用同位素稀释气相色谱-质谱联用(GC-MS)法,快速测定酱油中3-氯-1,2-丙二醇(3-MCPD)的含量。试样中加入3-氯-1,2-丙二醇的氘代同位素作为内标,经超声混匀后加入到自行填装的弗罗里硅土柱中,以乙醚洗脱,洗脱液经氮气吹干后在正己烷溶剂中进行衍生化,衍生化试剂采用七氟丁酰咪唑。GC-MS采用选择离子监测(SIM)模式进行定性定量分析。结果表明,本方法的添加回收率为95.0%~101.0%;相对标准偏差为3.2%~4.8%;检出限达到0.010mg/kg。本方法步骤简单,溶剂用量少,定性定量准确可靠。可快速测定酱油等调味品中3-氯-1,2-丙二醇的含量。

Rapid Determination of 3-Chloro-1,2-Propanediol in Soy Sauce by Gas Chromatography-Mass Spectrometry with Isotopic Dilution Method

The method using isotopic dilution and solid phase extraction (SPE) technique was established to determine the concentration of 3-chloro-1,2-propanediol in soy sauce by gas chromatography-mass spectrography ( GC-MS). Internal standard, 3-chloro-1,2-propanediol-d5 was added into soy sauce, after sonication, the mixture was transferred to a Florisil SPE column and eluted with ethyl ether. Evaporate the solution just to dry at room temperature under a stream of N2. 1.0 mL hexane and 0.05 mL heptafluorobutyry-limidazole were added immediately. GC-MS with SIM mode was applied to identify and quantitate. The recoveries ranged from 95.0%-101.0%. The relative standard deviation was 3.2%-4.8% with a detection limit of 0.010 mg/kg.