高效液相色谱-串联质谱法测定化妆品中10种抗生素

Simultaneous determination of 10 antibiotics in cosmetics by liquid chromatography tandem mass spectrometry

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 develop a liquid chromatography-tandem mass spectrometry（ LC-MS/MS） method for the simultaneous determination of minocycline hydrochloride,oxytetracycline dihydrate,tetracycline hydrochloride,chlortetracycline hydrochloride,doxycycline hyclate,chloramphenicol,metronidazole,lincomycin,clindamycin,clindamycin phosphate in cosmetics.Methods The samples were ultrasonically pretreated with methanol-0. 1 mol/L formic acid（ 1 ＋ 1,V/V） and the separation was carried out on an Agilent ZORBAX SB-C_（18）column（ 4. 6 mm × 75 mm,3. 5 μm） in a gradient elution mode,with 0. 2%formic acid aqueous solution as mobile phase A and 0. 2% formic acid methanol solution as mobile phase B. The flow rate was0. 5 ml/min; the injection volume was 5 μl and the column temperature was 30 ℃. The detection was accomplished in ESI＋mode. Results The linear range of the 10 antibiotics was within 20 ng/ml-2 000 ng/ml（ r 0. 998）,and the detection limit was less than 0. 04 μg/g,with the average recoveries in the range of 76. 8%-96. 9% at the spiked concentration of0. 50 μg/g,2. 0 μg/g and 16. 0 μg/g. The relative standard deviations（ RSDs） of the method were within 1. 5%-7. 2%.Conclusion The method is simple,rapid,selective,sensitive and accurate. It is suitable for the detection of the 10 antibiotics in cosmetics,such as minocycline hydrochloride.