摘要
目的:建立人血浆中克拉霉素测定的 HPLC-MS 法。方法:血浆经1mol·L^(-1)氢氧化钠溶液碱化后,用乙醚提取。采用 Zorbax SB-C_(18)(150mm×2.1 mm,5μm)分析柱,以乙腈-水-冰醋酸(60:40:0.05)为流动相,流速为0.4 mL·min^(-1);用HPLC-ESI^+-MS 法,选择性离子检测方法。质谱检测参数如下:干燥气流速13 L·min^(-1),干燥气温度350℃,雾化气压207kPa,毛细管电压3000 V,碎片电压150 V。选择检测的离子为 m/z 748.5(克拉霉素),m/z 837.5(罗红霉素)。结果:血浆中克拉霉素检测方法的线性范围为0.01～10μg·mL^(-1),最低检测限可达1.1 ng·mL^(-1)。血浆中克拉霉素的方法回收率为92.7%～99.4%,日内 RSD<5.1%,日间 RSD<3.6%。结论:本法灵敏,准确,可用于克拉霉素的药代动力学研究。
Objective：To develop a high performance liquid chromatography （HPLC） - mass spectrometry （MS） method for determination of clarithromycin in human plasma. Methods：The plasma was alkalised with 1 mol ·L^-1 sodium hydroxide solution and extracted with ether. The separation was performed on a Zorbax SB -C18 （150 mm × 2. 1 mm,5μm）. Analytical column using acetonitrile - water - acatic acid （60： 40：0.05 ） at a flow rate 0. 4 mL · min^-1 as the mobile phase. The analytes were detected by the positive electronic spray ionisation （ESI） - MS method under selectedion monitoring （SIM） mode. The MS detection parameters was ser as flows ： the dry gas flow was 13 L · min^-1, the drying gas temperature was 350℃, the nebulizer pressure was 207 kPa, the capillary voltage was 3000 V, the fragmentor was 150 V and the SIM ions were m/z 748.5 [ M ＋ H ] ^＋ for clarithromycin and m/z 837.5 [ M ＋ H ] ^＋ for roxithromycin. Results： The linear range of the plase concertration of clarithromycin was 0. 01 - 10 μg · mL^-1 and the limit of detection was 1.1 ng ·mL^-1. The relative recoveries of clarithremycin were 92. 7% -99. 4%. The RSDs of intra - day and inter - day were less than 5. 1% and 3.6% ,respectively. Conclusion：The method has high sensitivity and good selectivity ,it can be used for the pharmacokinetic research of clarithromycin.
出处
《药物分析杂志》
CAS
CSCD
北大核心
2005年第12期1433-1435,共3页
Chinese Journal of Pharmaceutical Analysis
关键词
克拉霉素
液相色谱-质谱联用
测定
血浆
方法学
clarithromycin, high performance liquid chromatography/mass spectrometry
