Lotfy Hayam M, Tawakkol Shereen M, Fahmy Nesma M, Shehata Mostafa A
Analytical Chemistry Department, Faculty of Pharmacy, Cairo University, Egypt.
Analytical Chemistry Department, Faculty of Pharmacy, Helwan University, Egypt.
Spectrochim Acta A Mol Biomol Spectrosc. 2015 Feb 5;136 Pt B:937-52. doi: 10.1016/j.saa.2014.09.117. Epub 2014 Oct 12.
Simultaneous determination of mixtures of lidocaine hydrochloride (LH), flucortolone pivalate (FCP), in presence of chlorquinaldol (CQ) without prior separation steps was applied using either successive or progressive resolution techniques. According to the concentration of CQ the extent of overlapping changed so it can be eliminated from the mixture to get the binary mixture of LH and FCP using ratio subtraction method for partially overlapped spectra or constant value via amplitude difference followed by ratio subtraction or constant center followed by spectrum subtraction spectrum subtraction for severely overlapped spectra. Successive ratio subtraction was coupled with extended ratio subtraction, constant multiplication, derivative subtraction coupled constant multiplication, and spectrum subtraction can be applied for the analysis of partially overlapped spectra. On the other hand severely overlapped spectra can be analyzed by constant center and the novel methods namely differential dual wavelength (D(1) DWL) for CQ, ratio difference and differential derivative ratio (D(1) DR) for FCP, while LH was determined by applying constant value via amplitude difference followed by successive ratio subtraction, and successive derivative subtraction. The spectra of the cited drugs can be resolved and their concentrations are determined progressively from the same ratio spectrum using amplitude modulation method. The specificity of the developed methods was investigated by analyzing laboratory prepared mixtures and were successfully applied for the analysis of pharmaceutical formulations containing the cited drugs with no interference from additives. The proposed methods were validated according to the ICH guidelines. The obtained results were statistically compared with those of the official or reported methods; using student t-test, F-test, and one way ANOVA, showing no significant difference with respect to accuracy and precision.
在不进行预先分离步骤的情况下,采用连续或逐次分辨技术,对盐酸利多卡因(LH)、特戊酸氟可的索(FCP)混合物在氯喹那多(CQ)存在下进行同时测定。根据CQ的浓度,重叠程度会发生变化,因此可使用比率减法从混合物中消除CQ,以得到LH和FCP的二元混合物,对于部分重叠光谱采用比率减法,对于严重重叠光谱,先通过幅度差得到恒定值,再进行比率减法,或者先采用恒定中心,再进行光谱减法。连续比率减法与扩展比率减法、常数乘法、导数减法与常数乘法相结合,光谱减法可用于分析部分重叠光谱。另一方面,严重重叠光谱可通过恒定中心以及针对CQ的新型方法即差分双波长(D(1) DWL)、针对FCP的比率差和差分导数比率(D(1) DR)进行分析,而LH则通过幅度差得到恒定值,然后进行连续比率减法以及连续导数减法来测定。所引用药物的光谱可通过幅度调制方法从同一比率光谱中进行分辨并逐步确定其浓度。通过分析实验室配制的混合物研究了所开发方法的特异性,并成功应用于含有所引用药物的药物制剂分析,不受添加剂干扰。所提出的方法按照国际协调会议(ICH)指南进行了验证。将所得结果与官方或报道方法的结果进行统计学比较;使用学生t检验、F检验和单因素方差分析,结果表明在准确性和精密度方面无显著差异。