气相色谱法测定生湿面制品中的乙二醇、 1,2-丙二醇和1,3-丙二醇

Determination of ethylene glycol, 1, 2-propanediol and 1, 3-propanediol in wet flour products by gas chromatography

中文关键词:  生湿面制品  乙二醇  丙二醇  气相色谱法

英文关键词:wet flour products  ethylene glycol  propanediol  gas chromatography

中文摘要:

      目的 建立对生湿面制品中乙二醇、1,2-丙二醇和1,3-丙二醇含量同时测定的气相色谱方法。方法 样品经粉碎, 加适量的海砂研磨成干粉状, 加入无水乙醇提取, 离心, 过滤后用气相色谱测定其中乙二醇、1,2-丙二醇和1,3-丙二醇的含量。采用石英毛细管色谱柱(HP-INNOWAX), 进样口为240 ℃, 分流比为20:1, 流速为1.0 mL/min, 程序升温为: 初始100 ℃, 维持4 min, 再以50 ℃/min升温至200 ℃, 维持8 min。检测器为氢火焰离子化检测器(FID), 检测器温度为280 ℃。结果 该方法在2.39~2500 μg/mL浓度范围内呈良好的线性关系, R2＞0.9993, 检出限为0.72~0.87 mg/kg。在5.0、10.0、50.0 mg/kg三个添加水平下, 平均回收率为87%~106% (n=6), 相对标准偏差(RSD)为1.3%~5.4% (n=6)。结论 该方法简便、快速、灵敏度好、准确度高, 所使用的试剂毒性小, 可同时检测大量样品, 能满足实际样品的检测要求。

英文摘要:

      Objective To establish a method of simultaneous determination of ethylene-glycol, 1,2- propanediol and 1,3-propanediol in wet flour products by gas chromatography. Methods The sample was shattered, ground into dry powder by adding proper amount of sea sands, extracted by anhydrous ethanol, and centrifuged, filtered, and detected the content of ethylene glycol, 1,2-propanediol and 1,3-propanediol by gas chromatography. By using silica capillary chromatography column (HP-INNOWAX), the temperature of the injection port was 240 ℃, the split ratio was 20:1, the flow rate was 1.0 mL/min, the programmed temperature was as follows: maintaining 100 ℃ for 4 min, and raising temperature to 200 ℃ at the rate of 50 ℃/min, then maintaining 8 min. The detector was hydrogen flame ionization detector and its temperature was 280 ℃. Results The method showed a good linearity over the range of 2.39~2500 μg/mL, R2＞0.9993, the detection limit was 0.72~0.87 mg/kg, the average recoveries were 87%~106% (n=6) and the relative standard derivations (RSD) were 1.3%~5.4% (n=6). Conclusion This method is simple, rapid, sensitive and accurate, and the reagents used have low toxicity, and it can test large quantity of samples simultaneously and satisfy the requirement of practical samples.