建立了直接提取结合液相色谱-电喷雾串联质谱同时测定化妆品中丹诺沙星、恩诺沙星、氟甲喹、恶喹酸、环丙沙星、沙拉沙星、萘啶酸、诺氟沙星、氧氟沙星等25种喹诺酮类药物的方法。样品经酸性乙腈提取和正己烷脱脂净化，采用 Poroshell EC-C18色谱柱分离，含0.1％甲酸的乙腈-水溶液为流动相进行梯度洗脱，电喷雾串联质谱正离子模式扫描，多反应监测（ MRM）模式检测，外标法定量。实验通过空白基质液配制标准溶液，以降低基质对离子化干扰造成的基质效应，25种喹诺酮类药物在1~200 mg／kg 范围内线性关系良好，相关系数（ r）在0.999以上。方法的检出限为1.0 mg／kg，在1、5、10 mg／kg 3个加标水平下，水、乳、霜型化妆品中加标回收率为87.4％~105％，相对标准偏差（ RSD）为4.54％~19.7％（ n=6）。结果表明，该方法简便、快速、准确，适用于化妆品中25种喹诺酮类药物的测定。
An analytical method was developed for the simultaneous determination of 25 quino-lones,including danofloxacin mesylate,enrofloxacin,flumequine,oxloinic acid,ciprofloxa-cin,sarafloxacin, nalidixic acid, norfloxacin, and ofloxacin etc in cosmetics using direct extraction and liquid chromatography-electrospray ionization tandem mass spectrometry( LC-ESI-MS/MS). Cosmetic sample was extracted by acidified acetonitrile,defatted by n-hexane and separated on Poroshell EC-C 18 column with gradient elution program using acetonitrile and water(both containing 0. 1% formic acid)as the mobile phases and analyzed by LC-ESI-MS/MS under the positive mode using multiple reaction monitoring( MRM). The interference of ma-trix was reduced by the matrix-matched calibration standard curve. The method showed good linearities over the range of 1—200 mg/kg for the 25 quinolones with good linear correlation coefficients( r≥0. 999). The method detection limit of the 25 quinolones was 1. 0 mg/kg,and the recoveries of all analytes in lotion,milky and cream cosmetics matrices ranged from 87. 4%to 105% at the spiked levels of 1,5 and 10 mg/kg with the relative standard deviations( RSD) of 4. 54%—19. 7%( n=6). The results indicated that this method is simple,fast and credible, and suitable for the simultaneous determination of the quinolones in the above three types of cosmetics.
参考文献
| [1] | 赵思俊;李存;江海洋;李炳玉;沈建忠.高效液相色谱检测动物肌肉组织中7种喹诺酮类药物的残留[J].分析化学,2007(6):786-790. |
| [2] | 李佩佩;郭远明;陈雪昌;张小军;梅光明;龙举.色谱法检测动物源食品中喹诺酮类药物残留研究进展[J].食品科学,2013(3):303-307. |
| [3] | 岳振峰;谢丽琪;陈小霞;吉彩霓;林秀云;侯乐锡;欧阳姗.牛奶中16种喹诺酮类药物残留量的高效液相色谱-串联质谱法测定[J].分析测试学报,2008(3):240-243. |
| [4] | 黄文静;洪建文;蒋忠军;赵艳婷.HPLC-DAD法检测化妆品中的氧氟沙星与环丙沙星[J].广州化工,2010(6):150-151,170. |
| [5] | 中华人民共和国卫生部.[J].化妆品卫生规范,2007 |
| [6] | 郑艳明;郭新东;冼燕萍;杜志峰;罗海英;吴玉銮;李慧勇.化妆品中7种氟喹诺酮类药物的反相高效液相色谱法测定[J].分析测试学报,2009(2):235-238. |
| [7] | 潘媛;牛华;程晓云;祝红昆;申南玉;李波;冯雷;珠娜;牛之瑞.高效液相色谱法检测六种氟喹诺酮类兽药残留前处理的优化[J].分析试验室,2011(5):69-72. |
| [8] | 祝颖;张虹.UPLC-MS/MS法同时检测水产品中喹诺酮类药物残留[J].中国食品学报,2010(2):206-213. |
| [9] | 包晓丽;任一平;张虹.超高效液相色谱-电喷雾串联四极杆质谱法检测牛奶中22种喹诺酮类抗菌素[J].分析化学,2009(3):389-394. |
| [10] | 吴小莲;向垒;莫测辉;李彦文;姜元能;严青云;吕旋;黄献培.超高效液相色谱-电喷雾串联质谱测定蔬菜中喹诺酮类抗生素[J].分析化学,2013(6):876-881. |
| [11] | 林峰;林海丹;吴映璇;王芳.LC-MS-MS测定烤鳗中4种氟喹诺酮药物残留量[J].分析测试学报,2004(5):43-47. |
| [12] | 李雅丽;郝晓蕾;冀宝庆;胥传来;沈崇钰;丁涛.HPLC-ESI-MS/MS测定动物性食品中19种喹诺酮类药物残留的研究[J].食品科学,2008(8):502-506. |
| [13] | 陈涛;陈安珍;杨钊.超高效液相色谱-串联质谱法测定动物源产品中11种喹诺酮类药物残留[J].药物分析杂志,2010(6):1087-1089. |
| [14] | GB/T 21312-2007.[S].,2007. |
| [15] | 杨方;庞国芳;刘正才;卢声宇;林永辉;余孔捷;李耀平;陈国南.液相色谱-串联质谱法检测水产品中15种喹诺酮类药物残留量[J].分析试验室,2008(12):27-33. |
| [16] | 岳振峰.食品中兽药残留检测指南[M].北京:中国标准出版社,2010 |
| [17] | 王丽;钟冬莲;陈光才;汤富彬;宋秋华;张建锋.固相萃取-高效液相色谱-串联质谱法测定畜禽粪便中的残留抗生素[J].色谱,2013(10):1010-1015. |
| [18] | 徐莉;徐志伟;陈文慧;梁振刚.UHPLC-MS/MS法快速测定水产品中17种磺胺和喹诺酮类药物[J].分析试验室,2012(9):114-117. |
| [19] | 曹鹏;牟妍;高飞;耿金培;张禧庆;隋涛;梁君妮;沙美兰;关丽丽.分散固相萃取-超高效液相色谱-串联质谱法同时检测火锅食材中11种喹诺酮类药物[J].色谱,2013(9):862-868. |
| [20] | 郑晶;黄晓蓉;郑俊超;陈彬;林杰.微生物抑制法与酶联免疫法检测鳗鱼中喹诺酮类药物残留的比较研究[J].中国卫生检验杂志,2006(1):79-81. |
| [21] | 卢晓蕊;霍任锋;许海东;沈虹.化妆品中喹诺酮类抗生素的液相色谱-串联质谱测定法[J].环境与健康杂志,2013(6):518-520. |
| [22] | 陈静;郑荣;季申;王柯.超高效液相色谱法同时测定化妆品中的19种喹诺酮类抗生素[J].分析化学,2013(6):931-935. |
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