柱前衍生-高效液相色谱法测定香精香料中硼酸和硼砂

香精香料样品中的硼酸经姜黄素的乙酸溶液在室温下进行衍生化,所得硼的衍生物用高效液相色谱法分析。选用Hypersil ODS2色谱柱(4.6mm×250mm,5μm)为固定相,以甲醇与0.012mol·L-1四丁基溴化铵(TBABr)溶液按体积比80比20混合所得溶液为流动相进行淋洗,于波长550nm处进行检测。根据硼砂在硫酸环境下定量转化成硼酸的原理间接测定硼砂。硼的色谱峰面积与其质量浓度在0.004～0.2 mg·L-1范围内呈线性关系,检出限(3s)为4.0×10-4 mg·L-1。在3个浓度水平下做加标回收试验,所得硼酸和硼砂的平均回收率分别在92.1%～106.6%和92.9%～107.1%之间。

HPLC Determination of Boric Acid and Borax in Essence and Perfume with Precolumn Derivatization

Boric acid in samples of essence and perfume was derivatized with curcumin(dissolved in acetic acid) at room temperature.The derivatized product of boron was used for HPLC analysis,using Hypersil ODS2 chromatographic column(4.6 mm×250 mm,5 μm) as stationary phase and mixtures of methanol and 0.012 mol·L-1 TBABr(80+20) as mobile phase.Based on the quantitative conversion of borax into boric acid in sulfuric acid medium,borax was determined by indirect determination of boric acid.Linear relationship was found between values of peak area determined at wavelength of 550 nm and mass concentration of boron in the range of 0.004-0.2 mg·L-1,with detection limit(3s) of 4.0×10-4mg·L-1.Tests for recovery were performed by standard addition method at 3 concentration levels;results of recovery of boric acid and borax found were in the ranges of 92.1%-106.6% and 92.9%-107.1% respectively.