液相色谱-串联质谱法测定婴儿乳粉中的抗坏血酸棕榈酸酯

Determination of ascorbyl palmitate in infant formula milk powder by liquid chromatography-tandem mass spectrometry

中文关键词:  抗坏血酸棕榈酸酯  液相色谱-串联质谱法  婴儿乳粉

英文关键词:ascorbyl palmitate  liquid chromatography-tandem mass spectrometry  infant formula milk powder

中文摘要:

      目的 建立液相色谱-串联质谱法(liquid chromatography-tandem mass spectrometry, LC-MS/MS)快速检测婴儿乳粉中抗坏血酸棕榈酸酯含量的方法。方法 样品经0.1%草酸乙醇溶液提取, 提取液用乙二胺-N-丙基硅烷(primary secondary amine, PSA)净化后经C18柱分离, 三重四极杆串联质谱检测。结果 抗坏血酸棕榈酸酯在0.02~0.5 μg/mL浓度范围内与峰面积呈良好的线性关系, 相关系数(r2)为0.9996, 检出限(S/N=3)为0.03 mg/kg, 定量限(S/N=10)为0.10 mg/kg。当添加浓度水平为0.5、1.0和10.0 mg/kg时, 平均回收率为90.0%~104.1%, 相对标准偏差(relative standard deviations, RSDs, n=6)为1.5%~2.7%。结论 本方法操作简便、快速、灵敏度高, 能够满足婴儿乳粉中抗坏血酸棕榈酸酯的检测要求。

英文摘要:

      Objective To establish a method for rapid detection of ascorbyl palmitate in infant milk powder by liquid chromatography-tandem mass spectrometry (LC-MS/MS). Methods The sample was extracted with 0.1% oxalic acid ethanol solution, and the extract was purified with ethylenediamine-N-propyl silane (primary secondary amine, PSA) and separated by a C18 column, and detected by a triple quadrupole tandem mass spectrometry. Results Ascorbyl palmitate had a good linear relationship with the peak area in the concentration range of 0.02?0.5 μg/mL, and the correlation coefficient (r2) was 0.9996. The limit of detection (LOD) (S/N=3) was 0.03 mg/kg, and the limit of quantitation (LOQ) (S/N=10) was 0.10 mg/kg. The mean recoveries at spiked levels of 0.5, 1.0 and 10.0 mg/kg were 90.0%?104.1%, with the relative standard deviations (RSDs) of 1.5%?2.7%(n=6). Conclusion This method is simple, rapid and sensitive, and can meet the requirements of detecting ascorbic palmitate in infant milk powder.