固相萃取反相高效液相色谱法测定人血清中洛美利嗪浓度
盐酸洛美利嗪,血清,高效液相色谱,固相萃取,药代动力学,,盐酸洛美利嗪，血清，高效液相色谱，固相萃取，药代动力学,摘要,关键词,1引言,2实验
摘 要 实验建立了固相萃取反相高效液相色谱法测定血清中洛美利嗪的浓度。采用Waters Oasis HLB 萃取小柱对血清样品进行固相萃取，以氟桂利嗪为内标，在Waters高效液相色谱系统上，C8为固定相，乙腈水(67∶33，含0.2%三乙胺，磷酸调节pH 至6.5)为流动相，流速：1 mL/min；检测波长: 223 nm；柱温：30℃；实验结果显示洛美利嗪和内标物洗脱时间分别为9.9 min和10.8 min，与血中内源性杂质得到良好分离。方法的相对回收率为99.6%～106.1%；绝对回收率为61.8%～86.5%；日内日间变异RSD范围分别为3.6%～53%和2.7%～6.9%；线性范围为5～320 μg/L(n=7, r=0.9998)。当S/N＝3时，洛美利嗪最低检出浓度可达5 μg/L。所建方法准确、灵敏，可满足血药浓度监测和药代动力学参数测试的需求。关键词 盐酸洛美利嗪，血清，高效液相色谱，固相萃取，药代动力学
Determination of Lomerizine in Human Serum by Reversed Phase High Performance Liquid Chromatography with
Solid Phase Extraction
Tang Jianlin, Zhou Shiwen*, Ying Yi, Wang Lu, Huang Yongpin
(Base for Drug Clinical Trial ,Xinqiao Hospital, Third Military Medical University, Chongqing 400037)
Abstract A reversed phase high performance liquid chromatography with solidphase extraction for the determination of lomerizine (LOZ) concentration in human serum was established. Using flunarizine(FOZ) as an internal standard (IS), solidphase extraction of human serum with waters oasis HLB column. The Loz and IS were separated on C8 column with acetonitrilewater (67∶33, 0.2% triethylamine, phosphatic acid adjust pH to 6.5) as the mobile phase, flow rate of 1 mL/min, detected at 223 nm, column temperature at 30 ℃. The linear range of calibration curve was within drug concentrations of 5-320 μg/L (n=7, r=0.9998). The lower limit of quantification(S/N＝3) was 5 μg/L. Relative recovery was 99.6%-106.1%, absolute recovery was 61.8%-86.5%. Intraand interassay RSD ranged from 3.6% to 5.3% and 2.7% to 6.9%, respectively. The method can be used for detection of lomerizine concentration in human serum and for estimation of pharmacokinetic parameters. ......
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