同位素内标-高效液相色谱质谱法测定婴幼儿配方乳粉中维生素B6和生物素

Simultaneous determination of vitamin B6 and biotin in infant formula milk powder by isotope internal standard coupled with high performance liquid chromatography mass spectrometry

中文关键词:  液相色谱串联质谱法  婴幼儿配方乳粉  维生素B6  生物素

英文关键词:high performance liquid chromatography tandem mass spectrometry  infant formula milk powder  vitamin B6  biotin

中文摘要:

      目的 建立同位素内标和高效液相色谱串联质谱法(high performance liquid chromatography tandem mass spectrometry, HPLC-MS/MS)同时测定婴幼儿配方乳粉中维生素B6含量(吡哆醛、吡哆醇和吡哆胺)和B7(生物素)的分析方法。方法 样品加入同位素内标后, 使用温水溶解, 并用高氯酸沉淀蛋白质, 上清液过滤后经HSS T3色谱柱分离, 三重四极杆质谱仪检测, 内标法定量。结果 在最优化条件下, 维生素B6和生物素分别在1.0~100 μg/L和0.10~10.0 μg/L范围内线性关系良好, 相关系数均大于0.998; 定量限分别为10.0 μg/100 g和1.0 μg/100 g。4种化合物的回收率为86.5%~97.9%, 相对标准偏差为3.0%~6.6%。质控样品检测结果表明该方法准确可靠。结论 该方法灵敏度高、净化效果好、定量准确, 适用于婴幼儿配方乳粉中维生素B6和维生素B7的检测。

英文摘要:

      Objective To establish a method for simultaneous determination of vitamin B6 (pyridoxal, pyridoxine, pyridoxamine) and vitamin B7 (biotin) in infant formula milk powder by isotope internal standard coupled with high performance liquid chromatography tandem mass spectrometry (HPLC-MS/MS). Methods After adding isotope internal standard, the sample was dissolved in warm water, and the protein was precipitated with perchloric acid. The supernatant was filtered and separated by HSS T3 chromatographic column, then detected by triple quadrupole mass spectrometer, and quantified by internal standard method. Results Under the optimal conditions, vitamin B6 and biotin had good linear relationships in the range of 1.0~100 μg/L and 0.10~10.0 μg/L, respectively, and the correlation coefficients were all greater than 0.998. The limits of quantification were 10.0 μg/100 g and 1.0 μg/100 g, respectively. The recoveries of the 4 compounds were 86.5%?97.9%, and the relative standard deviations were 3.0%?6.6%. The test results of quality control samples showed that the method was accurate and reliable. Conclusion This method has high sensitivity, good purification effect and accurate quantification, and is suitable for the detection of vitamin B6 and vitamin B7 in infant formula milk powder.