Dubey Nitin, Dubey Nidhi, Mandhanya Mayank, Kumar Jain Dinesh
Department of Industrial Quality Assurance and Sophisticated Instrumentation, College of Pharmacy, IPS Academy, Indore 452012 (MP), India.
Department of Pharmaceutical Analysis, School of Pharmacy, Devi Ahilya University, Indore 452011 (MP), India.
J Pharm Anal. 2012 Dec;2(6):478-483. doi: 10.1016/j.jpha.2012.04.003. Epub 2012 Apr 25.
Prevention of cross contamination with active pharmaceutical ingredients is crucial and requires special attention in pharmaceutical industries. Current method validation describes the determination of Nabumetone (NAB) residue on a stainless steel surface using swab sampling with a sensitive HPLC-DAD analysis. The acceptance limit was decided as 2 μg swab per 100 cm. Cotton swabs impregnated with extraction solution were used to determine residual drug content. Recoveries were 90.88%, 91.42%, and 92. 21% with RSD ranging from 2.2% to 3.88% at three concentration levels. Residual concentration was found to be linear in the range of 0.1-4.56 μg/mL, when estimated using a Phenomenex Luna C (25 cm×5 μm×4.6 mm i.d.) column at 1.0 mL/min flow rate and 230 nm. The mobile phase consisted of a mixture of methanol:acetonitrile:water (55:30:15, v/v/v). The LOD and LOQ for NAB were found to be 0.05 and 0.16 μg/mL, respectively. The validated method was found to be simple, selective and sensitive for demonstration of cleaning validation of NAB residues on a stainless steel surface.
防止与活性药物成分发生交叉污染至关重要，在制药行业需要特别关注。当前的方法验证描述了使用拭子采样结合灵敏的高效液相色谱 - 二极管阵列检测（HPLC - DAD）分析来测定不锈钢表面的萘丁美酮（NAB）残留量。验收限设定为每100平方厘米拭子2微克。用浸渍有萃取溶液的棉拭子来测定残留药物含量。在三个浓度水平下，回收率分别为90.88%、91.42%和92.21%，相对标准偏差（RSD）在2.2%至3.88%之间。当使用菲罗门Luna C（25厘米×5微米×4.6毫米内径）色谱柱，流速为1.0毫升/分钟，检测波长为230纳米时，残留浓度在0.1 - 4.56微克/毫升范围内呈线性关系。流动相由甲醇：乙腈：水（55:30:15，v/v/v）的混合物组成。萘丁美酮的检测限（LOD）和定量限（LOQ）分别为0.05和0.16微克/毫升。已验证的方法对于证明不锈钢表面萘丁美酮残留的清洁验证而言简单、具有选择性且灵敏。
