摘要:
建立了一种柱前衍生化高效液相色谱法(HPLC)测定荞麦中D-手性肌醇(D-CI)含量的方法,对衍生化试剂及方法的重复性、稳定性、精密性及加标回收率进行了考察。得到衍生化条件为:苯甲酰氯0.2 mL,吡啶0.6 mL,反应温度70℃,反应时间60 min;色谱条件为:C18柱(4.6 mm×250 mm,5 μm),以乙腈和超纯水为流动相进行梯度洗脱,流速为1.0 mL/min,柱温30℃,UV检测波长230 nm。结果表明,荞麦中的D-CI获得了很好的分离,D-CI在0.004~0.04 mg/mL内线性相关性好,R2为0.999,加标回收率为98.40%~100.67%,所建立的方法稳定、灵敏、重现性好,可用于测定荞麦中D-CI含量定量分析。
Abstract:
A method was established for the determination of D-chiro-inositol(D-CI)by pre-column derivatization HPLC. Repeatability,stability,precision and added standard recovery of the method and the derivatization conditions were investigated. Derivatization conditions were as follows:0.2 mL of benzoyl chloride,0.6 mL of pyridine,reaction temperature 70℃,reaction time of 60 min. Chromatographic conditions were as follows:using C18 column(4.6 mm×250 mm,5 μm),with acetonitrile and ultrapure water as mobile phrase in gradient elution,flow rate of 1.0 mL/min,column temperature of 30℃,and UV detection wavelength of 230 nm. The results showed that D-CI of buckwheat won good separation by the method,and the method got a good linear relationship of D-CI concentration and peak area at a range of 0.004~0.04 mg/mL with 0.999 of R2 and the recovery was 98.40%~100.67%. So the method was stable,sebsitive,good reproducibility,and could be used to determine the content of D-CI from buckwheat.
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