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首页> 外文期刊>CHROMATOGRAPHY >Enantioselective Determination of Synephrine in Health Food Products by Liquid Chromatography/Time-of-Flight Mass Spectrometry
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Enantioselective Determination of Synephrine in Health Food Products by Liquid Chromatography/Time-of-Flight Mass Spectrometry

机译：液相色谱/飞行时间质谱法对健康食品中的术治疗术治疗的映射性测定

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An enantioselective analytical method for the determination of synephrine, an ingredient in health food, by liquid chromatography/time-of-flight mass spectrometry (LC/TOF-MS) was developed. By derivatizing synephrine with FMOC and using TCI Chiral MB-S as the chiral column, FMOC-synephrine enantiomers were well separated. The electrospray ionization (ESI) negative mode was adopted for TOF-MS measurement. Good linearity (r > 0.999) was obtained in the concentration range of 0.5 to 50 μg/mL. The limit of detection (LOD, S /N = 3) and the limit of quantification (LOQ, S /N > 10) were 0.25 μg/mL and 0.5 μg/mL, respectively. The intra-day and inter-day accuracy of synephrine enantiomers at the LOQ level (0.5 μg/mL), the intermediate concentration level (10 μg/mL), and the high concentration level (50 μg/mL) ranged from 90.0 to 107.4%. The intra-day and inter-day precisions were ≤ 9.24% and ≤ 10.63%, respectively. As a result of analyzing synephrine-containing health foods using this method, approximately half of the products showed high optical purity with 80–100% enantiomeric excess of the l -isomer. In contrast, nearly 20% of the products contained racemate with 0–50% enantiomeric excess, and variations in optical purity were observed for the products. It was speculated that the l -isomer could be converted into the d -isomer during the manufacturing process.
机译：开发了一种对嗜疗法测定的映选择性分析方法，液相色谱/飞行时间质谱（LC / TOF-MS）的健康食品中的成分。通过用FMOC衍生同步管和使用TCI手性MB-S作为手性柱，FMOC-同步向映异构体分开很好。采用电喷雾电离（ESI）负模式进行TOF-MS测量。在0.5至50μg/ ml的浓度范围内获得良好的线性度（ r> 0.999）。检测限（LOD， S / I> N = 3）和定量限（LOQ， S / I> N> 10）为0.25μg/ mL和0.5μg/ ml，分别。 LOQ水平（0.5μg/ ml），中间浓度水平（10μg/ ml）和高浓度水平（50μg/ ml）的日期和日间准确度，高浓度水平（50μg/ ml）为90.0至107.4 ％。日内和日间间诊断分别≤9.24％和≤10.63％。由于使用该方法分析含有血管含健康食品的结果，大约一半的产品显示出高光学纯度，具有80-100％对映体过量的 L-ISOmer。相比之下，近20％的产物含有0-50％对映体过量的外消旋物，并且对产品的光学纯度的变化观察到。据推测，在制造过程中，可以将 L-isOmer转化为 D-isOmer。

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