Hussain Saleh, Patel Harshvardhan, Tan Aimin
Anapharm, 120 Newkirk Road, Richmond Hill, ON L4C 9S7, Canada.
Bioanalysis. 2009 Jun;1(3):529-35. doi: 10.4155/bio.09.47.
Liquid-liquid extraction has been widely used for the analysis of rosuvastatin due to its many attractive features, such as low cost and clean extract. However, manual transfer of the organic phase poses a challenge, particularly when a batch size is large. To overcome the challenge, a simple automated high-throughput (192 samples per batch) liquid-liquid extraction method with short (3.0-min) chromatographic run time was proposed. Rosuvastatin was separated using a gradient on a reversed-phase C18 column and detected in the multiple reaction monitoring made with a mass transition of m/z 482.3→258.2 amu.
The assay exhibited a linear range from 50 to 25000 pg/ml (r ≥ 0.9976). The intra- and inter-day accuracy ranged from 98.16 to 103.84% and 101.18 to 103.95%, respectively. The intra- and inter-day precision ranged from 0.70 to 6.17% and 2.19 to 5.07%, respectively.
Finally, the validated method was successfully applied to bioequivalence studies.
液-液萃取因其诸多吸引人的特性，如低成本和提取物纯净，已被广泛用于瑞舒伐他汀的分析。然而，手动转移有机相带来了挑战，尤其是当批量较大时。为克服这一挑战，提出了一种简单的自动化高通量（每批192个样品）液-液萃取方法，其色谱运行时间短（3.0分钟）。使用反相C18柱上的梯度分离瑞舒伐他汀，并在多反应监测中以m/z 482.3→258.2 amu的质量跃迁进行检测。
该测定法的线性范围为50至25000 pg/ml（r≥0.9976）。日内和日间准确度分别为98.16%至103.84%和101.18%至103.95%。日内和日间精密度分别为0.70%至6.17%和2.19%至5.07%。
最后，该验证方法成功应用于生物等效性研究。
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