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目的建立化妆品中盐酸美满霉素、二水土霉素、盐酸四环素、盐酸金霉素、盐酸多西环素、氯霉素、甲硝唑、林可霉素、克林霉素及克林霉素磷酸酯10种抗生素的高效液相色谱-串联质谱检测方法。方法样品经甲醇+0.1 mol/L甲酸溶液(1+1,V/V)涡旋超声提取后,经Agilent ZORBAX SB-C_(18)色谱柱(4.6 mm×75 mm,3.5μm)分离,以0.2%甲酸水溶液为流动相A,0.2%甲酸的甲醇溶液为流动相B,梯度洗脱;流速为0.5 ml/min;进样量为5μl;柱温为30℃。串联质谱正离子模式检测。结果 10种抗生素线性范围为20 ng/ml~2 000 ng/ml(r>0.998),检出限<0.04μg/g,在0.50μg/g、2.0μg/g及16.0μg/g 3种加标浓度下,10种抗生素平均回收率为76.8%~96.9%,RSD为1.5%~7.2%。结论该方法快速简便,具有良好的选择性、灵敏度及准确度,适用于化妆品中盐酸美满霉素等10种抗生素的测定。
Objective To establish Cosmetic composition of minocycline hydrochloride, water oxytetracycline, tetracycline hydrochloride, chlortetracycline hydrochloride, doxycycline hyclate, chloramphenicol, metronidazole, lincomycin, clindamycin and clindamycin High Performance Liquid Chromatography - Tandem Mass Spectrometry Detection of 10 Kinds of Antibiotics. Methods The samples were vortexed by methanol + 0.1 mol / L formic acid solution (1 + 1, V / V) and separated on an Agilent ZORBAX SB-C 18 column (4.6 mm × 75 mm, 3.5 μm) 0.2% formic acid aqueous solution as mobile phase A, 0.2% formic acid in methanol as mobile phase B, gradient elution; flow rate 0.5 ml / min; injection volume 5μl; Tandem mass spectrometry positive mode detection. Results The linear range of the 10 antibiotics was 20 ng / ml ~ 2000 ng / ml (r> 0.998). The detection limit was lower than 0.04μg / g. The antibiotics at 0.50μg / g, 2.0μg / g and 16.0μg / The average recoveries of 10 antibiotics were 76.8% ~ 96.9% and RSD were 1.5% ~ 7.2% at standard concentration. Conclusion The method is rapid and simple, has good selectivity, sensitivity and accuracy and is suitable for the determination of 10 antibiotics such as minocycline hydrochloride in cosmetics.