色谱

色谱 ›› 2012, Vol. 30 ›› Issue (06): 641-646.DOI: 10.3724/SP.J.1123.2012.02024

• 技术与应用 • 上一篇    

高效液相色谱法同时测定祛痘产品中6种抗生素及甲硝唑

陆军*, 庞燕军, 李彦博, 王超   

  1. 辽宁省食品药品检验所, 辽宁 沈阳 110023
  • 收稿日期:2012-02-16 修回日期:2012-03-26 出版日期:2012-06-28 发布日期:2012-06-20
  • 通讯作者: 陆军,高级工程师,研究方向为食品研发与检验、化妆品质量分析与检验和药物质量分析与检验. Tel: (024)25449296, E-mail: zsc671225@163.com.

Simultaneous determination of 6 antibiotics and metronidazole in acne removal products by high performance liquid chromatography

LU Jun*, PANG Yanjun, LI Yanbo, WANG Chao   

  1. Liaoning Institute for Food and Drug Control, Shenyang 110023, China
  • Received:2012-02-16 Revised:2012-03-26 Online:2012-06-28 Published:2012-06-20
  • Contact: lu-lu LU

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摘要： 建立了一种高效液相色谱-二极管阵列检测器(HPLC-DAD)同时测定祛痘产品中6种抗生素(盐酸美满霉素、土霉素、盐酸四环素、盐酸金霉素、盐酸多西环素和氯霉素)及甲硝唑的分析方法。样品用甲醇提取,采用Agilent ZORBAX SB-C18色谱柱(250 mm×4.6 mm, 5 μm)分离;以甲醇、乙腈和0.002 mol/L草酸为流动相进行梯度洗脱,流速0.8 mL/min;柱温20 ℃,检测波长268 nm,进样量10 μL,外标法定量。结果表明,6种抗生素及甲硝唑在1～30 mg/L范围内呈良好的线性关系,相关系数(r)均不低于0.9970；方法检出限为1.1～1.2 μg/g；高、中、低(5、10、20 mg/L) 3个添加水平下的回收率为91.9%～107.7%,相对标准偏差(RSD)为0.13%～1.74%。应用该方法对祛痘产品进行检验,15%的样品中检出甲硝唑。该方法具有灵敏、准确、快速、分离效果好的优点,适用于祛痘产品中6种抗生素及甲硝唑的检测。

关键词: 高效液相色谱, 甲硝唑, 抗生素, 祛痘产品；化妆品

Abstract: An analytical method for the simultaneous determination of 6 antibiotics (minocycline, oxytetracycline, tetracycline hydrochloride, chlorotetracycline hydrochloride, doxycycline hydrochloride and chloramphenicol) and metronidazole in acne removal products of cosmetic was established using high performance liquid chromatography (HPLC). The drugs in the sample were extracted with methanol. The separation was performed on an Agilent ZORBAX SB-C18 column (250 mm×4.6 mm, 5 μm) at 20 ℃ with methanol, acetonitrile and 0.002 mol/L oxalic acid solution as mobile phases with gradient elution at a flow rate of 0.8 mL/min. The detection was performed by a diode array detector (DAD) at 268 nm. The injection volume was 10 μL. The quantification was performed by external standard method. The calibration curves showed good linearity within the range of 1-30 mg/L with the correlation coefficients no less than 0.9970. The detection limits were in the range of 1.1-1.2 μg/g. The recoveries were between 91.9% and 107.7% in three spiked levels of 5, 10 and 20 mg/L with the relative standard deviations (RSDs) of 0.13%-1.74%. The method was used in the analysis of acne removal products, and metronidazole was found in 15% of the total test samples. The method is rapid, sensitive, accurate, effective in separation, and can be used in the determination of the six antibiotics and metronidazole in acne removal products.

Key words: acne removal products, antibiotics, cosmetics, metronidazole, high performance liquid chromatography (HPLC)

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