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采用4-(N-氯甲酰甲基-N-甲基氨基)-7-硝基-2,1,3-苯并恶二唑柱前衍生化,结合高效液相色谱-荧光检测法简单测定护肤液中的邻苯基苯酚。

Simple determination of o-phenylphenol in skin lotion by high-performance liquid chromatography coupled with fluorescence detection after pre-column derivatization with 4-(N-chloroformylmethyl-N-methylamino)-7-nitro-2,1,3-benzoxadiazole.

作者信息

Higashi Yasuhiko, Konno Kazunori

出版信息

J Cosmet Sci. 2015 Mar-Apr;66(2):129-37.

Abstract

o-Phenylphenol (OPP) in skin lotion was quantitated by high-performance liquid chromatography coupled with fluorescence detection after pre-column derivatization with 4-(N-chloroformylmethyl-N-methylamino)-7-nitro-2,1,3-benzoxadiazole (NBD-COCl) in borate buffer (pH 8.5) at room temperature for 2 min. The column [150 mm x 3.0 mm internal diameter (i.d.)], which contained 5 μm particles of C18 packing material, was eluted at room temperature (flow rate: 0.5 ml/min) with mobile phase prepared by addition of acetonitrile (550 ml) to 450 ml of Milli-Q water containing trifluoroacetic acid (0.1 v/v%). 2-Hydroxyfluorene was used as an internal standard. The retention times of NBD-CO-OPP and NBD-CO-IS derivatives were 16.2 and 22.2 min, respectively. The calibration plot was linear in the range of 0.01-0.2 μg/ml with an r2 value of 0.9960, and the lower limit of detection was 0.003 μg/ml (at a signal-to-noise ratio of 3:1; absolute amount of 12 pg/20 μl injection). The coefficient of variation was less than 8.8%. Contents of OPP in three skin lotions were determined with the present system, and the recovery from spiked samples was satisfactory.

摘要

皮肤乳液中的邻苯基苯酚(OPP)通过高效液相色谱法结合荧光检测进行定量。在硼酸盐缓冲液(pH 8.5)中,于室温下用4-(N-氯甲酰基甲基-N-甲基氨基)-7-硝基-2,1,3-苯并恶二唑(NBD-COCl)进行柱前衍生化2分钟。色谱柱[150 mm×3.0 mm内径(i.d.)],填充有5μm粒径的C18填料,在室温下(流速:0.5 ml/min)用流动相洗脱,流动相由向450 ml含0.1%(v/v)三氟乙酸的超纯水加入550 ml乙腈配制而成。2-羟基芴用作内标。NBD-CO-OPP和NBD-CO-IS衍生物的保留时间分别为16.2分钟和22.2分钟。校准曲线在0.01 - 0.2 μg/ml范围内呈线性,r2值为0.9960,检测下限为0.003 μg/ml(信噪比为3:1;进样20 μl时绝对量为12 pg)。变异系数小于8.8%。用本系统测定了三种皮肤乳液中OPP的含量,加标样品的回收率令人满意。

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