色谱

色谱 ›› 2012, Vol. 30 ›› Issue (07): 684-689.DOI: 10.3724/SP.J.1123.2012.02039

• 研究论文 • 上一篇    下一篇

高效液相色谱-串联质谱法同时检测口腔卫生产品中抗生素类药物

周卫军1*, 谢正福1, 邵琳智2   

  1. 1. 广东省食品药品监督管理局审评认证中心, 广东 广州 510080; 2. 广东检验检疫技术中心, 广东 广州 510623
  • 收稿日期:2012-02-27 出版日期:2012-07-28 发布日期:2012-07-19
  • 通讯作者: 周卫军,硕士,主管药师,主要从事药品注册审评、药物分析工作. Tel: (020)37886285, E-mail: wejoy@tom.com.
  • 基金资助:

    国家检验检疫行业标准制定计划项目(No.2009B099).

Determination of antibiotics in oral hygiene products by high performance liquid chromatography-tandem mass spectrometry

ZHOU Weijun1*, XIE Zhengfu1, SHAO Linzhi2   

  1. 1. Guangdong Food and Drug Administration Center for Evaluation & Certification, Guangzhou 510080, China; 2. Guangdong Inspection and Quarantine Technology Center, Guangzhou 510623, China
  • Received:2012-02-27 Online:2012-07-28 Published:2012-07-19

PDF

296

被引次数

7

摘要： 采用高效液相色谱-串联质谱技术,建立了口腔卫生产品(牙膏及漱口水)中5类共13种抗生素的同时检测方法。分析物包括5种四环素类、3种大环内酯类、2种喹诺酮类、1种β-内酰胺类和2种林可胺类抗生素。样品经0.1%(体积分数,下同)甲酸溶液-乙腈(95:5, v/v)提取,高速离心并过滤,稀释后采用C18色谱柱(150 mm×2.1 mm, 5 μm)分离,以0.1%甲酸溶液-乙腈为流动相梯度洗脱,采用电喷雾离子源串联质谱,在正离子扫描方式下以多反应监测(MRM)模式检测,外标法定量。13种抗生素类药物在5.0～50.0 μg/L质量浓度范围内线性关系良好(相关系数大于0.99),定量限为10.0 mg/kg。两种基质(牙膏及漱口水)样品在10、20和100 mg/kg 3个加标水平下的平均回收率为80.1%～115%,相对标准偏差为0.94%～8.69%。该方法准确可靠、方便快捷,适用于口腔卫生产品中抗生素类药物的定性定量分析。

关键词: 高效液相色谱-串联质谱法, 抗生素, 口腔卫生产品

Abstract: A high performance liquid chromatography-tandem mass spectrometry (HPLC-MS/MS) method was developed for simultaneous determination of 13 antibiotics in oral hygiene products, including five tetracyclines, three macrolides, two quinolones, one β-lactam and two lincosamides. The sample was extracted with 0.1% (volume percentage, same hereinafter) formic acid-acetonitrile (95:5, v/v), then centrifuged, filtered and diluted. The target compounds were separated on a C18 column (150 mm×2.1 mm, 5 μm) with a gradient elution of 0.1% formic acid and acetonitrile as the mobile phases, and detected by tandem mass spectrometry in positive electrospray ionization and multiple reaction monitoring (MRM) mode. The quantification of 13 antibiotics was performed by the external standard method. The calibration curves showed good linearity in the range of 5.0~50.0 μg/L with detection limits of 10.0 mg/kg. The recoveries of antibiotics in mouthwash and toothpaste samples at the three spiked levels of 10, 20 and 100 mg/kg were in the range of 80.1%~115% with the relative standard deviations in the range of 0.94%~8.69%. This method is accurate, reliable, simple, and suitable for the analysis of antibiotics in oral hygiene products.

Key words: antibiotics, oral hygiene products, high performance liquid chromatography-tandem mass spectrometry (HPLC-MS/MS)