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Development of Isotope Dilution-Liquid Chromatography/Tandem Mass Spectrometry as a Candidate Reference Method for the Determination of Folic Acid in Infant Milk Formula

机译:同位素稀释液色谱/串联质谱法在婴儿配方奶粉中叶酸测定中的候选参考方法的发展

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An isotope dilution-liquid chromatography/tandem mass spectrometric method was developed as a candidate reference method for the accurate determination of folic acid in infant milk formula. Sample was spiked with ~(13)C_5-folic acid and then extracted with phosphate buffer (pH 6) solution. The extract was further cleaned up by deproteinization followed by a C~(18) solid-phase extraction cartridge. The extract was analyzed by using LC/ ESI/MS/MS with selectively monitoring the collisionaHy induced dissociation channels of m/z 442 -> m/z 295 and m/z 447 -> m/z 295, which are the neutral glutamyl loss from the [M+H]~+ ions of folic acid and ~(13)C_5-folic acid, respectively. LC/MS/MS chromatograms showed substantially reduced background from chemical noises compared to LC/MS chromatograms. Repeatability and reproducibility studies showed that the LC/MS/ MS method is a reliable and reproducible method which can provide less than 1.5 relative percentage of method precision.
机译:同位素稀释液相色谱/串联质谱法被开发为准确测定婴儿配方奶粉中叶酸的候选参考方法。样品中加入〜(13)C_5-叶酸,然后用磷酸盐缓冲液(pH 6)溶液萃取。通过脱蛋白,然后用C〜(18)固相萃取柱进一步纯化萃取液。通过使用LC / ESI / MS / MS分析提取物,并选择性监测碰撞引起的解离通道m / z 442-> m / z 295和m / z 447-> m / z 295,这是中性谷氨酰丢失叶酸和〜(13)C_5叶酸的[M + H]〜+离子。与LC / MS色谱图相比,LC / MS / MS色谱图显示出来自化学噪声的背景显着减少。重复性和重现性研究表明,LC / MS / MS方法是一种可靠且可重现的方法,相对于方法精度,其相对百分比不到1.5。

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