1. 嘉应学院梅州师范分院
2. 广州质量监督检测研究院
3. 中国广州分析测试中心
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Quantitative Determination of 4 Nitroimidazoles in Acne Cosmetics by Gas Chromatography-Mass Spectrometry. [J]. 34(8):911-916(2015)
建立了同时测定祛痘化妆品中4种硝基咪唑类化合物(甲硝唑、奥硝唑、洛硝唑和塞克硝唑)的气相色谱-质谱联用(GC-MS)分析方法。样品用碳酸钠溶液溶解后以乙酸乙酯提取,经浓缩和(或)正己烷除脂后,用N,O-双(三甲基硅烷基)乙酰胺衍生,样液经DB-5 MS(30 m×0.25 mm×0.25 μm)毛细管色谱柱分离,GC-MS的选择离子监测(SIM)模式检测,以保留时间和特征离子比值定性,同位素内标法定量。结果表明,4种硝基咪唑类化合物在0.10~5.0 mg/L范围内线性关系良好,相关系数均不小于0998;方法检出限(S/N=3)为0.05~0.10 mg/kg;在祛痘水和祛痘膏样品中进行3个水平的加标实验,平均回收率为85.6%~104%,相对标准偏差(RSD,n=6)为2.9%~6.5%。实际样品检测表明本方法准确可靠,适用于祛痘化妆品中硝基咪唑类化合物的同时测定。
A new method was developed for the simultaneous determination of four nitroimidazoles,e.g.metronidazole(MNZ),ornidazole(ONZ),ronidazole(RNZ) and secnidazole(SNZ), in acne cosmetics by gas chromatography-mass spectrometry(GC-MS).The samples were firstly diluted with sodium carbonate solution and then extracted with ethyl acetate.The extract was subsequently concentrated and/or the fat in which was wiped off with n-hexane.Finally,four nitroimidazoles were derivatised using N,O-bis(trimethylsilyl)-acetamide as derivating agent,and separated on a DB-5 MS capillary chromatographic column(30 m × 0.25 mm × 0.25 μm).The target compounds were identified by GC-MS with retention time and ratio of the characteristic ions under selected ion monitoring(SIM) mode,and quantified by the internal standard method.The result indicated that 4 analytes had good linear relationships(r2≥0.998) in the concentrations of 0.10-5.0 mg/L.The detection limits of target compounds for this method(LODs,S/N=3) ranged from 0.05 mg/kg to 0.10 mg/kg.The recoveries of four nitroimidazoles at three spiked levels in acne cream and acne water samples were in the range of 85.6%-104%,with relative standard deviations(RSDs,n= 6) of 2.9%-6.5%.The real sample analysis showed that this accurate and precise method could be applied in the simultaneous determination of four nitroimidazoles in acne cosmetics.
气相色谱-质谱联用法祛痘化妆品硝基咪唑类化合物
gas chromatography-mass spectrometry(GC-MS)acne cosmeticsnitroimidazoles
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