气相色谱-质谱法检测婴幼儿配方乳粉中6种丁香酚类物质含量

Determination of 6 kinds of eugenols in infant formula milk powder by gas chromatography-mass spectrometry

中文关键词:  气相色谱-质谱法  配方乳粉  丁香酚  甲基丁香酚  异丁香酚  顺式-甲基异丁香酚  乙酸丁香酚酯  乙酰基异丁香酚

英文关键词:gas chromatography-mass spectrometry  formula milk powder  eugenol

中文摘要:

      目的 建立简便高效的气相色谱-质谱法测定婴幼儿配方乳粉中6种丁香酚类物质。方法 样品经乙腈超声提取后, 使用乙腈饱和的正己烷净化除脂, 弃去正己烷, 提取乙腈浓缩定容至1 mL。采用DB-1701色谱柱分离, 不分流进样, 进样量1 μL。采用选择离子监测模式进行气相色谱-质谱法测定, 外标法定量。结果 6种丁香酚类物质在20~500 ng/mL内呈良好的线性关系, 本方法中6种丁香酚类化合物检出限均为0.007 mg/kg, 定量限均为0.02 mg/kg。在牛乳粉和羊乳粉两种基质样品中, 6种丁香酚类物质的3个不同浓度水平的加标平均回收率在97.3%~105.0%之间, 相对标准偏差(relative standard deviation, RSD)在0.3%~3.7%之间。结论 该方法前处理操作简便、快捷, 检测方法灵敏度高、稳定性好, 满足国家标准要求。为建立婴幼儿配方乳粉中6种丁香酚类物质检测的国家标准或方法提供参考依据。

英文摘要:

      Objective To establish a simple and efficient method for the determination of 6 kinds of eugenols in infant formula milk powder by gas chromatography-mass spectrometry. Methods After ultrasonic extraction with acetonitrile, the sample was purified and degreased using acetonitrile saturated n-hexane. The n-hexane was discarded, and acetonitrile was extracted and concentrated to a volume of 1 mL. DB-1701 chromatographic column was used to separate without splitting the sample, with an injection volume of 1 μL. Ion monitoring mode for gas chromatography-mass spectrometry determination and external standard method for quantification was used. Results The 6 kinds of eugenols showed a good linear relationship within the range of 20–500 ng/mL, the limit of detection of the 6 kinds of eugenol compounds in this method was 0.007 mg/kg, and the limit of quantitation was 0.02 mg/kg. In 2 matrix samples of milk powder and sheep milk powder, the average recoveries of 6 kinds of eugenols at 3 different concentration levels were between 97.3% and 105.0%, the relative standard deviation (RSD) was between 0.3% and 3.7%. Conclusion The pretreatment operation of this method is simple and fast, and the detection method has high sensitivity and good stability, meeting the requirements of national standards, in order to provide reference basis for establishing national standards or methods for the detection of 6 kinds of eugenols in infant formula milk powder.