在酸性条件下,生活饮用水化学处理剂中六价铬与二苯碳酰二肼进行衍生反应,以磷酸二氢钾缓冲溶液和乙腈-丙酮(体积比为1∶1)混合溶液为流动相,衍生物经Atlantis T3 C 18分析柱分离,在540 nm波长下检测。六价铬在0.001 mg/L^0.500 mg/L范...在酸性条件下,生活饮用水化学处理剂中六价铬与二苯碳酰二肼进行衍生反应,以磷酸二氢钾缓冲溶液和乙腈-丙酮(体积比为1∶1)混合溶液为流动相,衍生物经Atlantis T3 C 18分析柱分离,在540 nm波长下检测。六价铬在0.001 mg/L^0.500 mg/L范围内线性良好,方法检出限为5.00 mg/kg,标准样品6次测定结果的RSD为0.9%~3.5%,实际样品加标回收率为76.0%~98.5%。展开更多
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 qualit...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).展开更多
文摘在酸性条件下,生活饮用水化学处理剂中六价铬与二苯碳酰二肼进行衍生反应,以磷酸二氢钾缓冲溶液和乙腈-丙酮(体积比为1∶1)混合溶液为流动相,衍生物经Atlantis T3 C 18分析柱分离,在540 nm波长下检测。六价铬在0.001 mg/L^0.500 mg/L范围内线性良好,方法检出限为5.00 mg/kg,标准样品6次测定结果的RSD为0.9%~3.5%,实际样品加标回收率为76.0%~98.5%。
文摘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).
