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尿液、血浆和腹膜透析液中雷尼替丁的自动固相萃取及高效液相色谱测定法

Automated solid-phase extraction and high-performance liquid chromatographic determination of ranitidine from urine, plasma and peritoneal dialysate.

作者信息

Karnes H T, Opong-Mensah K, Farthing D, Beightol L A

机构信息

Department of Pharmacy and Pharmaceutics, Medical College of Virginia, Richmond 23298-0001.

出版信息

J Chromatogr. 1987 Nov 27;422:165-73. doi: 10.1016/0378-4347(87)80449-8.

Abstract

Ranitidine is an H2-receptor antagonist primarily used to treat peptic ulcer. The present automated solid-phase extraction technique involves sorbent conditioning of a cyano (CN) cartridge with 0.5 ml of methanol and 1.0 ml of extraction buffer (0.005 M phosphate, pH 9). Plasma samples were applied by passing 1.0 ml of plasma through the cartridge and subsequently washing with 2 ml of the extraction buffer. Appropriate larger volumes of dialysate were used to concentrate ranitidine onto the cartridge so that the amount eluted was increased to within detectable limits. Urine samples were deluted with distilled water to decrease the ranitidine concentration to within the range of the standard curve. The high-performance liquid chromatographic method (mobile phase 88-89% of 0.02 M phosphate buffer pH 3 and 11-12% of methanol; Spherisorb phenyl cartridge column, 10 cm X 0.46 cm I.D., 5 micron particle diameter, flow-rate 1.1 ml/min; detection at 228 nm) is sensitive to 2 ng/ml in 1 ml of sample. The internal standard of choice was determined to be n-propionylprocainamide as compared to cimetidine and lidocaine. The method was cost-efficient, rapid and simple due to the automated sample processing. The coefficient of variation on replicate assays was less than 10% over all concentrations studied. Recoveries were between 97 and 110%, and the method was linear over the range 1.90-687.20 with a mean correlation coefficient of 0.999.

摘要

雷尼替丁是一种H2受体拮抗剂,主要用于治疗消化性溃疡。目前的自动化固相萃取技术包括用0.5毫升甲醇和1.0毫升萃取缓冲液(0.005M磷酸盐,pH9)对氰基(CN)柱进行吸附剂预处理。通过将1.0毫升血浆通过柱子并随后用2毫升萃取缓冲液洗涤来施加血浆样品。使用适当较大体积的透析液将雷尼替丁浓缩到柱子上,以便洗脱的量增加到可检测限度内。尿液样品用蒸馏水稀释以将雷尼替丁浓度降低到标准曲线范围内。高效液相色谱法(流动相为88 - 89%的0.02M pH3磷酸盐缓冲液和11 - 12%的甲醇;Spherisorb苯基柱,10cm×0.46cm内径,5微米粒径,流速1.1ml/min;在228nm处检测)对1毫升样品中的2ng/ml敏感。与西咪替丁和利多卡因相比,确定选择的内标为正丙酰普鲁卡因酰胺。由于采用了自动化样品处理,该方法具有成本效益、快速且简单。在所有研究浓度下,重复测定的变异系数小于10%。回收率在97%至110%之间,该方法在1.90 - 687.20范围内呈线性,平均相关系数为0.999。

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