HPLC-PDA检测祛痘除螨类化妆品中非法添加盐酸米诺环素方法的建立
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摘要
目的建立用高效液相色谱-二极管阵列检测法(HPLC-PDA)检测祛痘除螨类化妆品中非法添加的盐酸米诺环素,以打击化妆品中非法添加禁限物质的不法行为。方法采用Waters Symmetry C18(5μm,4.6 mm×250 mm)色谱柱;以醋酸铵缓冲盐溶液(取醋酸铵15 g、氯化钾10 g与乙二胺四乙酸二钠5 g,加水溶解并稀释成1 000 ml)-乙腈(70∶30)为流动相等度洗脱;流速为1.0 ml/min;柱温为25℃;检测波长280 nm;用PDA检测,以保留时间和紫外光谱图定性,峰面积定量。结果盐酸米诺环素在1~100μg/ml范围内与峰面积呈良好的线性关系,相关系数为1.000 0,检出限为0.1μg/ml,方法的回收率为88.5%~98.5%,RSD为1.0%~1.5%(n=6)。结论该方法特异性强,灵敏度高,准确可靠,适用于不同基质样品中盐酸米诺环素的检测。
[Objective]To establish a HPLC-PDA method for detecting the minocycline hydrochloride illegally added in acne removal cosmetics, crack down the delict of illegally adding the prohibited and restricted substances in the cosmetics.[Methods]The separation was performed on a Waters Symmetry C18(5 μm,4.6 mm×250 mm)column using ammonium acetate buffer solution(dissolve 15 g ammonium acetate,10 g potassium chloride and 5 g EDTA-2Na in water,and dilute to 1 000 ml)-acetonitrile(70∶30) as mobile phase with the detection wavelength at 280 nm,flow rate of 1.0 ml/min and column temperature25 ℃. PDA was used for detecting,retention time and UV spectrum were used for qualitative analysis,and peak area was used for quantification.[Results]The calibration curve of minocycline hydrochloride showed good linearity within the range of 1-100μg/ml(r=1.000 0). The detection limit was 0.1 μg/ml. The recovery rate was 88.5%-98.5%,the RSD was 1.0%-1.5%(n=6).[Conclusion]This method is specific,sensitive,accurate and reliable,which is applicable for the detection of minocycline hydrochloride in different matrix samples.
[Objective]To establish a HPLC-PDA method for detecting the minocycline hydrochloride illegally added in acne removal cosmetics, crack down the delict of illegally adding the prohibited and restricted substances in the cosmetics.[Methods]The separation was performed on a Waters Symmetry C18(5 μm,4.6 mm×250 mm)column using ammonium acetate buffer solution(dissolve 15 g ammonium acetate,10 g potassium chloride and 5 g EDTA-2Na in water,and dilute to 1 000 ml)-acetonitrile(70∶30) as mobile phase with the detection wavelength at 280 nm,flow rate of 1.0 ml/min and column temperature25 ℃. PDA was used for detecting,retention time and UV spectrum were used for qualitative analysis,and peak area was used for quantification.[Results]The calibration curve of minocycline hydrochloride showed good linearity within the range of 1-100μg/ml(r=1.000 0). The detection limit was 0.1 μg/ml. The recovery rate was 88.5%-98.5%,the RSD was 1.0%-1.5%(n=6).[Conclusion]This method is specific,sensitive,accurate and reliable,which is applicable for the detection of minocycline hydrochloride in different matrix samples.
引文
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[2]王亚斐,杨正生,刁慕戈,等.扶正消毒饮联合美满霉素治疗中重度痤疮疗效观察[J].中成药,2014,36(4):883-884
[3]刘华良,杨润,李放,等.化妆品中7种常见抗生素的超高效液相色谱测定法[J].环境与健康杂志,2009,26(5):453-454.
[4]刘华良,李放,杨润,等.超高效液相色谱-串联质谱法分析化妆品中的常见抗生素及甲硝唑[J].色谱,2009,27(1):50-53.
[5]赵同刚.化妆品卫生规范[M].北京:军事医学科学出版社,2007,257-258
[6]杨艳伟,朱英,张卫强.化妆品中7种抗生素及地塞米松磷酸钠和水杨酸的高效液相色谱测定法[J].环境与健康杂志,2006,23(3):264-266.
[7]武婷,王超,李楠.高效液相色谱法测定化妆品中九种禁用四环素类抗生素的方法研究[J].分析试验室,2007,26(8):52-54.
[8]吴大南,郑和辉.高效液相色谱法测定化妆品中四种抗生素[J].中国卫生检验杂志,2012,22(12),2837-2838,2841
[9]吴宏伟,郭伟斌,苏智阳,等.盐酸米诺环素HPLC的流动相探讨[J].中国药品标准,2003,4(6):52-54
[10]国家药典委员会.中国药典2010版[M].二部.北京:中国医药科技出版社,2010:697-699.