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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

[Simultaneous determination of 6 antibiotics and metronidazole in acne removal products bt high performance liquid chromatography].

作者信息

Lu Jun, Pang Yanjun, Li Yanbo, Wang Chao

机构信息

Liaoning Institute for Food and Drug Control, Shenyang 110023, China.

出版信息

Se Pu. 2012 Jun;30(6):641-6. doi: 10.3724/sp.j.1123.2012.02024.

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 x 4.6 mm, 5 microm) at 20 degrees C 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 microL. 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 0.997 0. The detection limits were in the range of 1.1 - 1.2 microg/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.

摘要

采用高效液相色谱法(HPLC)建立了一种同时测定祛痘化妆品中6种抗生素(米诺环素、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。样品中的药物用甲醇提取。在Agilent ZORBAX SB-C18色谱柱(250 mm×4.6 mm,5μm)上,于20℃以甲醇、乙腈和0.002 mol/L草酸溶液为流动相进行梯度洗脱,流速为0.8 mL/min,采用二极管阵列检测器(DAD)在268 nm波长处进行检测。进样量为10μL,采用外标法定量。校准曲线在1 - 30 mg/L范围内呈良好线性,相关系数不小于0.997 0。检测限为1.1 - 1.2μg/g。在5、10和20 mg/L三个加标水平下,回收率为91.9% - 107.7%,相对标准偏差(RSD)为0.13% - 1.74%。该方法用于祛痘产品分析,发现15%的总测试样品中含有甲硝唑。该方法快速、灵敏、准确,分离效果好,可用于测定祛痘产品中的6种抗生素及甲硝唑。

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