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研究建立了祛痘化妆品中4种硝基呋喃类抗生素(呋喃妥因、呋喃唑酮、呋喃它酮及呋喃西林)的高效液相色谱测定方法。样品以乙腈+甲醇(70+30,V/V)混合溶液进行超声提取,提取液经微孔滤膜过滤后,滤液由XTerra MS C18(4.6 mm×250 mm,5μm)色谱柱分离,以15 mmol/L乙酸铵溶液和乙腈为流动相进行梯度洗脱,外标法定量。疑似阳性样品采用高效液相色谱-质谱/质谱法确证。4种化合物在各自线性范围内线性良好,呋喃妥因、呋喃唑酮及呋喃西林的定量限为5 mg/kg,呋喃它酮的定量限为7.5 mg/kg。在低、中、高3个添加浓度水平下,4种物质的的平均回收率在85.0%~99.6%,相对标准偏差(RSD)为2.1%~9.5%。
A method for the determination of four kinds of nitrofurans antibiotics (nitrofurantoin, furazolidone, furandamone and nitrofurazone) in acne cosmetic was established. The sample was extracted with acetonitrile + methanol (70 + 30, V / V) mixed solution and the extract was filtered through a microporous membrane. The filtrate was separated on a XTerra MS C18 column (4.6 mm × 250 mm, 5 μm) mmol / L ammonium acetate solution and acetonitrile as the mobile phase gradient elution, external standard method. Suspected positive samples were confirmed by high performance liquid chromatography-mass spectrometry / mass spectrometry. The four compounds showed good linearity in their respective linear ranges with a quantitative limit of 5 mg / kg for nitrofurantoin, furazolidone and nitrofurazone, and a limit of quantification for furanketone of 7.5 mg / kg. The average recoveries of the four substances ranged from 85.0% to 99.6% with relative standard deviations (RSDs) ranging from 2.1% to 9.5% at low, medium and high concentration levels.