Mohamed Gehad Genidy, Rizk Mahmoud Sabry, Zaky Frag Eman Yousry
Chemistry Department, Faculty of Science, Cairo University, Giza, 12613, Egypt.
Iran J Pharm Res. 2015 Summer;14(3):701-14.
The purpose of this investigation was directed to propose sensitive, accurate and reproducible methods of analysis that can be applied to determine distigmine bromide (DTB), cyclopentolate hydrochloride (CPHC), diaveridine hydrochloride (DVHC) and tetrahydrozoline hydrochloride (THHC) drugs in pure form and pharmaceutical preparations via charge-transfer complex formation with 7,7,8,8-tetracyanoquinodimethane (TCNQ) and tetracyanoethylene (TCNE) reagents. Spectrophotometric method involve the addition a known excess of TCNQ or TCNE reagents to DTB, CPHC, DVHC and THHC drugs in acetonitrile, followed by the measurement of the absorbance of the CT complexes at the selected wavelength. The reaction stoichiometry is found to be 1:1 [drug]: [TCNQ or TCNE]. The absorbance is found to increase linearly with concentration of the drugs under investigation which is corroborated by the correlation coefficients of 0.9954-0.9981. The system obeys Beer's law for 6-400, 20-500, 1-180 and 60-560 µg mL(-1) and 80-600, 10-300, 1-60 and 80-640 µg mL(-1) for DTB, CPHC, DVHC and THHC drugs using TCNQ and TCNE reagents, respectively. The apparent molar absorptivity, sandell sensitivity, the limits of detection and quantification are also reported for the spectrophotometric method. Intra- and inter-day precision and accuracy of the method were evaluated as per ICH guidelines. The method was successfully applied to the assay of DTB, CPHC, DVHC and THHC drugs in formulations and the results were compared with those of a reference method by applying Student's t and F-tests. No interference was observed from common pharmaceutical excipients.
本研究旨在提出灵敏、准确且可重现的分析方法,该方法可通过与7,7,8,8 - 四氰基对苯二醌二甲烷(TCNQ)和四氰基乙烯(TCNE)试剂形成电荷转移络合物,用于测定纯品及药物制剂中的溴化双斯的明(DTB)、盐酸环喷托酯(CPHC)、盐酸二氨藜芦啶(DVHC)和盐酸四氢唑啉(THHC)。分光光度法是在乙腈中向DTB、CPHC、DVHC和THHC药物中加入已知过量的TCNQ或TCNE试剂,然后在选定波长下测量电荷转移络合物的吸光度。发现反应化学计量比为1:1 [药物] : [TCNQ或TCNE]。在所研究药物浓度范围内,吸光度与药物浓度呈线性增加,相关系数为0.9954 - 0.9981,证实了这一点。使用TCNQ和TCNE试剂时,该体系分别对DTB、CPHC、DVHC和THHC药物在6 - 400、20 - 500、1 - 180和60 - 560 μg mL⁻¹以及80 - 600、10 - 300、1 - 60和80 - 640 μg mL⁻¹范围内符合比尔定律。还报道了分光光度法的表观摩尔吸光系数、桑德尔灵敏度、检测限和定量限。按照国际协调会议(ICH)指南评估了该方法的日内和日间精密度及准确度。该方法成功应用于制剂中DTB、CPHC、DVHC和THHC药物的含量测定,并通过应用学生t检验和F检验将结果与参考方法的结果进行比较。未观察到常见药用辅料的干扰。