4-(N,N -二甲氨基磺酰基)-7-(N -氯甲酰甲基- N -甲氨基)-2,1,3-苯并恶二唑柱前衍生- hplc -荧光分析香味雾中覆盆子酮的改进方法

Y. Higashi
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引用次数: 2

摘要

树莓酮{RK, 4-(4-羟基苯基)丁醇-2- 1}在结构上类似于4-(4-羟基苯基)-2-丁醇,它会导致消费者皮肤上的白皮病。因此,在化妆品质量评价中测量是很重要的。最近建立了4-肼-7-硝基-2,1,3-苯并恶二唑肼柱前衍生法测定香味雾中RK含量的hplc -荧光法。然而,衍生化条件(80°C, 20 min)是苛刻的。本研究以4-(N,N-二甲氨基磺酰基)-7-(N-氯甲酰基甲基-N-甲氨基)-2,1,3-苯并恶二唑(DBD-COCl)为原料,采用改进的柱前衍生法测定RK。DBD-CO-RK衍生物从反相ODS柱洗脱,在440 nm激发和543 nm发射波长下检测。在室温下衍生3 min, DBD-CO-RK衍生物的保留时间为16.8 min,标准曲线在0.05 ~ 2.5 μg/mL范围内呈良好的线性关系,相关系数(r2)值为0.9988。检测下限为0.01 μg/mL(绝对量0.3 pmol)。变异系数均小于10.0%。香雾(1.00 mL)中RK含量为1.20±0.08 mg(范围:1.10 ~ 1.31 mg, n = 5),回收率为91.8±5.4%;范围:84.2 ~ 98.2%,n = 5)。
本文章由计算机程序翻译,如有差异,请以英文原文为准。
Improved Method for Determination of Raspberry Ketone in Fragrance Mist by HPLC-Fluorescence Analysis after Pre-Column Derivatization with 4-( N,N -Dimethylaminosulfonyl)-7-( N -chloroformylmethyl- N -methylamino)-2,1,3-benzoxadiazole
Raspberry ketone {RK, 4-(4-hydroxyphenyl)butan-2-one} is structurally resembles 4-(4-hydroxyphenyl)-2-butanol, which causes leukoderma on consumers’ skin. Therefore, it is important to measure in cosmetics for quality assessment. Very recently, an HPLC-fluorescence method for determination of RK in a fragrance mist by pre-column derivatization with 4-hydrazino-7-nitro-2,1,3-benzoxadiazole hydrazine was established. However, the derivatization conditions (80°C, 20 min) were severe. In this study, an improved pre-column derivatization with 4-(N,N-dimethylaminosulfonyl)-7-(N-chloro-formylmethyl-N-methylamino)-2,1,3-benzoxadiazole (DBD-COCl) is presented by HPLC-fluorescence method for determination of RK. The DBD-CO-RK derivative was eluted from a reversed-phase ODS column, and detected with excitation at 440 nm and emission at 543 nm. Derivatization was performed at room temperature for 3 min. The retention time of DBD-CO-RK derivative was 16.8 min. The standard curve was linear in the range of 0.05 to 2.5 μg/mL, with a correlation coefficient (r2) value of 0.9988. The lower limit of detection was 0.01 μg/mL (absolute amount of 0.3 pmol). The coefficients of variation were less than 10.0%. The content of RK in fragrance mist (1.00 mL) was 1.20 ± 0.08 mg (range, 1.10 to 1.31 mg, n = 5). Recovery tests were satisfactory (91.8 ± 5.4%; range, 84.2 to 98.2%, n = 5).
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