高效液相色谱-二极管阵列检测法测定化妆品中6种抗生素

Determination of six antibiotics in cosmetics by high performance liquid chromatography with diode array detector detection

目的建立用高效液相色谱-二极管阵列检测器(HPLC-PDA)检测化妆品中抗生素二水土霉素、盐酸四环素、盐酸金霉素、盐酸多西环素、氯霉素及甲硝唑的方法。方法采用Waters Symmetry C18(4.6 mm×250 mm,5μm)色谱柱;以0.01 mol/L草酸溶液(pH=2.0)-乙腈-甲醇为流动相,梯度洗脱;检测波长:268 nm;流速:1.0 ml/min;柱温为25℃。以保留时间和紫外光谱图定性,峰面积定量。结果 6组分在1μg/ml^100μg/ml范围内与峰面积呈良好的线性关系,相关系数均>0.9995,检出限均为0.1μg/ml,方法的回收率为83.2%~107.9%,RSD为0.5%~4.4%(n=6)。结论该方法特异性强,适用于不同基质的化妆品,准确可靠,可用于实际样品的检测。

Objective To establish a HPLC- DAD method for determination of six antibiotics including oxytetracycline dihydrate,tetracycline hydrochloride,chlorotetracycline hydrochloride,doxycycline hydrochloride,chloramphenicol and metronidazole in cosmetics. Methods The gradient elution was performed using a Waters Symmetry C18（ 4.6 mm ×250 mm,5 μm） as chromatographic column,using 0. 01 mol /L oxalic acid solution（ pH = 2. 0）- acetonitrile- methanol as mobile phase with the detection wavelength at 268 nm,flow rate of 1. 0 ml /min and column temperature 25 ℃. Retention time and UV spectrum were used for qualititation,and peak area was used for quantitation. Results The calibration curves of six antibiotics showed good linearity within the range of 1 μg /ml - 100 μg /ml with the correlation coefficients above 0. 9995. The detection limits were0. 1 μg /ml. The recovery rates were 83. 2% - 107. 9% with RSD of 0. 5% - 4. 4%（ n = 6）. Conclusion The method is specific,accurate and reliable and is applicable for the analysis of different matrix cosmetics.