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高效液相色谱法同时测定化妆品中8种呋喃香豆素并采用液相色谱-串联质谱法进行验证

[Simultaneous determination of eight furocoumarines in cosmetics by high performance liquid chromatography and verification by liquid chromatography-tandem mass spectrometry].

作者信息

Ma Huijuan, Ma Qiang, Li Wentao, Meng Xianshuang, Li Jingrui, Bai Hua, Jiao Yang, Zhang Xiaoli

机构信息

Chinese Academy of Inspection and Quarantine, Beijing 100123, China.

出版信息

Se Pu. 2013 May;31(5):416-22. doi: 10.3724/sp.j.1123.2012.12006.

Abstract

A method using high performance liquid chromatography (HPLC) and liquid chromatography-tandem mass spectrometry (LC-MS/MS) was developed for the simultaneous determination of eight furocoumarines (8-hydroxypsoralen, psoralen, isopsoralen, 8-methoxypsoralen, 5-methoxypsoralen, trioxsalen, imperatorin and isoimperatorin) in cosmetics. The cosmetic samples, including cream, lotion, shampoo, powder and lipstick, were supersonically extracted with appropriate solvents. The extract was centrifuged, and the supernatant was filtered through a membrane, and then separated on an Agilent Zorbax SB-Phenyl chromatographic column (250 mm x 4.6 mm, 5 microm) by gradient elution at a flow rate of 1.0 mL/min with methanol-acetonitrile-water as mobile phases. The column temperature was set at 30 degrees C. The wavelength of detection was 250 nm. The limits of quantification (LOQs) were 0.25 mg/kg for 8-hydroxypsoralen and 0.5 mg/kg for psoralen, isopsoralen, 8-methoxypsoralen, 5-methoxypsoralen, trioxsalen, imperatorin and isoimperatorin. The recoveries at three spiked levels were in the range of 85.0% - 105.8% with the relative standard deviations (RSDs) of 0.41% - 7.90%. The intra-day precision (n=6) was less than 1%, and the inter-day precision (n = 6) was less than 2% for the peak areas of the eight furocoumarines in a mixed standard solution. The method is accurate, simple, rapid and suitable for the determination of the eight furocoumarines in various cosmetic samples.

摘要

建立了一种采用高效液相色谱(HPLC)和液相色谱 - 串联质谱(LC - MS/MS)同时测定化妆品中8种呋喃香豆素(8 - 羟基补骨脂素、补骨脂素、异补骨脂素、8 - 甲氧基补骨脂素、5 - 甲氧基补骨脂素、三甲沙林、欧前胡素和异欧前胡素)的方法。化妆品样品,包括面霜、乳液、洗发水、香粉和口红,用适当的溶剂进行超声提取。提取物离心后,上清液通过膜过滤,然后在Agilent Zorbax SB - Phenyl色谱柱(250 mm×4.6 mm,5μm)上以1.0 mL/min的流速进行梯度洗脱分离,流动相为甲醇 - 乙腈 - 水。柱温设定为30℃。检测波长为250 nm。8 - 羟基补骨脂素的定量限(LOQs)为0.25 mg/kg,补骨脂素、异补骨脂素、8 - 甲氧基补骨脂素、5 - 甲氧基补骨脂素、三甲沙林、欧前胡素和异欧前胡素的定量限为0.5 mg/kg。三个加标水平下的回收率在85.0% - 105.8%范围内,相对标准偏差(RSDs)为0.41% - 7.90%。混合标准溶液中8种呋喃香豆素峰面积的日内精密度(n = 6)小于1%,日间精密度(n = 6)小于2%。该方法准确、简单、快速,适用于各种化妆品样品中8种呋喃香豆素的测定。

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