Zhang Haixia, Choi Hoo-Kyun
College of Pharmacy, Chosun University, 501-759, Gwangju, Korea.
Anal Bioanal Chem. 2008 Nov;392(5):947-53. doi: 10.1007/s00216-008-2333-0. Epub 2008 Aug 27.
A simple cloud-point extraction method for the determination of meloxicam in human serum was developed. Meloxicam was extracted from serum sample after adding 1 mL of 3% (v/v) Triton X-114 aqueous solution in the presence of 1M HCl and 60 mg NaCl. The meloxicam, present in the surfactant-rich phase, was enriched again with acetonitrile. Tenoxicam was used as the external standard. The separation was achieved on a C18 analytical column with a mobile phase consisting of aqueous acetic acid (1%, v/v) and acetonitrile (54:46, v/v). UV detection was performed at 360 nm. The response was linear over the range 45-2000 ng mL(-1) in human serum, and intra- and interday precisions of less than 15.0% were obtained. The relative error was within +/-3.0%. The recoveries of meloxicam were larger than 92.0%. The method was compared with liquid-liquid extraction. The results showed that the new method has a considerable LOQ and higher recoveries but poorer precision than liquid-liquid extraction, which exhibited poor recoveries of less than 86.0%, precisions of less than 5.0% and relative errors of less than 7.0%. The method was used for the determination of meloxicam in healthy human volunteers.
建立了一种用于测定人血清中美洛昔康的简单浊点萃取法。在1M盐酸和60mg氯化钠存在下,加入1mL 3%(v/v)Triton X-114水溶液后,从血清样品中萃取美洛昔康。存在于富表面活性剂相中的美洛昔康再用乙腈富集。替诺昔康用作外标。在C18分析柱上进行分离,流动相由乙酸水溶液(1%,v/v)和乙腈(54:46,v/v)组成。在360nm处进行紫外检测。在人血清中,响应在45 - 2000 ng mL(-1)范围内呈线性,日内和日间精密度均小于15.0%。相对误差在±3.0%以内。美洛昔康的回收率大于92.0%。将该方法与液 - 液萃取法进行比较。结果表明,新方法的检测限相当,回收率较高,但精密度比液 - 液萃取法差,液 - 液萃取法的回收率小于86.0%,精密度小于5.0%,相对误差小于7.0%。该方法用于健康人体志愿者中美洛昔康的测定。