HPLC-DAD法测定家兔关节液中头孢唑林钠的含量

doi:10.5246/jcps.2014.09.083

中国药学(英文版) ›› 2014, Vol. 23 ›› Issue (9): 649-653.DOI: 10.5246/jcps.2014.09.083

HPLC-DAD法测定家兔关节液中头孢唑林钠的含量

李静¹, 林微微¹, 李玳², 敖英芳^2*, 杨海松¹, 凌笑梅^1*

1. 北京大学医学部药学院药物分析教研室, 北京 100191
2. 北京大学第三医院运动医学研究所, 北京 100191

收稿日期:2014-04-06 修回日期:2014-05-04 出版日期:2014-09-23 发布日期:2014-05-14
通讯作者: Tel.: 86-10-82802414, 86-10-82267390
基金资助:
National Natural Science Foundation (Grant No. 81373372) and Specialized Research Fund for the Doctoral Program of Higher Education of China (Grant No. 20110001110021 and 20130001110059).

A validated HPLC method for the determination of cefazolin sodium level in rabbit synovial fluid

Jing Li¹, Weiwei Lin¹, Dai Li², Yingfang Ao^2*, Haisong Yang¹, Xiaomei Ling^1*

1. Department of Pharmaceutical Analysis, School of Pharmaceutical Sciences, Peking University Health Science Center, Beijing 100191, China
2. Institute of Sports Medicine, The Third Hospital of Peking University, Beijing 100191, China

Received:2014-04-06 Revised:2014-05-04 Online:2014-09-23 Published:2014-05-14
Contact: Tel.: 86-10-82802414, 86-10-82267390
Supported by:
National Natural Science Foundation (Grant No. 81373372) and Specialized Research Fund for the Doctoral Program of Higher Education of China (Grant No. 20110001110021 and 20130001110059).

摘要/Abstract

摘要：

本实验建立了一种灵敏且专属的HPLC-DAD测定家兔关节液中头孢唑林钠的方法。用乙腈沉淀关节液中的蛋白质, 安替比林作为内标。样品在戴安U3000高效液相色谱仪上操作, 并用菲罗门Luna C₁₈ (150 mm×4.60 mm, 5 μm, 100 A)柱分离, 流动相为0.1%甲酸水和乙腈, 流速为1 mL/min, 检测波长为272nm, 柱温为25 ºC。在1.0-100.0 μg/mL范围内, 头孢唑林钠和内标安替比林的峰面积比值与浓度线性关系良好(r²= 0.9999), 最低检测限为(LOD, S/N = 3)为0.07 μg/mL,最低定量限(LOD, S/N = 10)为0.22 μg/mL。头孢唑林钠回收率(低、中、高浓度)分别为124.6%、117.8%、100.6% (RSD% = 1.9%, 4.0%, 1.1%, n = 5)。日内和日间精密度在0.5%-2.7%。本实验建立的家兔关节液中头孢唑林钠HPLC-DAD分析方法简便、灵敏且可靠。此方法可以应用于家兔关节液中头孢唑林钠的测定。

关键词: 头孢唑林钠, 家兔关节液, 高效液相色谱

Abstract:

A sensitive and specific high performance liquid chromatography method was established for measuring cefazolin sodium level in rabbit synovial fluid.Acetonitrile was used to precipitate proteins and antipyrine was used as internal standard. Samples were analyzed on a Dionex Ultimate U3000 HPLC system equipped with Phenomenex Luna C₁₈ column (150 mm×4.60 mm, 5 μm, 100 A). The mobile phase consisted of acetonitrile and 0.1% formic acid in water. The flow rate was 1 mL/min. The detectionwavelength was set at 272 nm. The column temperature was maintained at 25 ºC.The calibration curve was linear in the range of 1.0-100.0 μg/mL(r² = 0.9999). The limit of detection (LOD, S/N = 3) was 0.07 μg/mL. The limit of quantitation (LOD, S/N = 10) was 0.22 μg/mL. The recovery of cefazolin sodium (low, medium and high) was 124.6%, 117.8%, and 100.6% (RSD% = 1.9%, 4.0%, 1.1%, n = 5), respectively. The intra-day and inter-day precision values were in the range of 0.5%-2.7%.The method was simple, sensitive and reliable. It can be used for the quantitative determination of cefazolin sodium in rabbit synovial fluid.

Key words: Cefazolin sodium, Rabbit synovial fluid, HPLC

中图分类号:

R917

Supporting:

李静, 林微微, 李玳, 敖英芳, 杨海松, 凌笑梅. HPLC-DAD法测定家兔关节液中头孢唑林钠的含量[J]. 中国药学(英文版), 2014, 23(9): 649-653.

Jing Li, Weiwei Lin, Dai Li, Yingfang Ao, Haisong Yang, Xiaomei Ling. A validated HPLC method for the determination of cefazolin sodium level in rabbit synovial fluid[J]. Journal of Chinese Pharmaceutical Sciences, 2014, 23(9): 649-653.

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HPLC-DAD法测定家兔关节液中头孢唑林钠的含量

A validated HPLC method for the determination of cefazolin sodium level in rabbit synovial fluid

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