Analytical Chemistry Department, Faculty of Pharmacy, Misr International University, Km 28 Misr-Ismailia Road, Cairo, Egypt.
Pharmaceutical Analytical Chemistry Department, Faculty of Pharmacy, Kasr El Aini, Cairo University, Cairo, 11562, Egypt.
Sci Rep. 2024 Sep 18;14(1):21775. doi: 10.1038/s41598-024-71046-6.
A selective, precise, and accurate reversed HPLC method has been developed and validated for simultaneous separation and determination of two veterinary drugs, dipyrone and hyoscine, in their combined dosage form in the presence of their official impurities, namely 4-aminoantipyrine and tropic acid, in addition to the formulated preservative: phenol. The linearity range was found to be (1.00-35.00 µg/mL) for dipyrone and (2.50-50.00 µg/mL) for hyoscine. It exhibited a satisfactory linearity regression R (0.9999) for both drugs with LOD 0.22 µg/mL and 0.72 µg/mL and LOQ 0.65 µg/mL and 2.19 µg/mL for dipyrone and hyoscine, respectively. Additionally, the two cited drugs were also determined in the presence of dipyrone active metabolite 4-aminoantipyrine using diclofenac as an internal standard in bovine urine. The linearity range was found to be (15-75 µg/mL) for dipyrone, (2.5-60 µg/mL) for hyoscine, and (2.5-60 µg/mL) for 4-aminoantipyrine with linearity regression R (0.9999-0.9998). The LLOQ (15, 2.5, 2.5 µg/mL), LQC (45, 7.5, 7.5 µg/mL), MQC (55, 25, 25 µg/mL), and HQC (60, 50 50 µg/mL) were determined for dipyrone, hyoscine and 4-aminoantipyrine, respectively. UV detection was carried out at 220 nm. The method was validated according to the ICH guidelines, as well as according to FDA guidelines for determining both drugs in bioanalytical matrices and both proved accuracy and precision. A statistical comparison was made between the results obtained and those obtained by the reported method, showing no significant difference in accuracy and precision at p = 0.05. The suggested method was proved eco-friendly through a greenness assessment using two different tools (The analytical eco-scale scored 83, and the AGREE-Analytical Greenness Metric approach scored 0.83). The suggested method can be used in the routine work of quality control labs, screening for drug abuse, and ensuring clean sport for horse racing.
建立并验证了一种选择性、精确性和准确性高的反相高效液相色谱法,用于在存在其官方杂质(即 4-氨基安替比林和托品酸)以及规定防腐剂:苯酚的情况下,同时分离和测定两种兽用药物:双氯芬酸和氢溴酸东莨菪碱在其复方制剂中的含量。双氯芬酸的线性范围为(1.00-35.00μg/mL),氢溴酸东莨菪碱的线性范围为(2.50-50.00μg/mL)。两种药物的线性回归 R(0.9999)均令人满意,双氯芬酸和氢溴酸东莨菪碱的检测限分别为 0.22μg/mL 和 0.72μg/mL,定量限分别为 0.65μg/mL 和 2.19μg/mL。此外,还使用双氯芬酸作为内标,在牛尿中测定了两种被引用药物的活性代谢物 4-氨基安替比林。双氯芬酸的线性范围为(15-75μg/mL),氢溴酸东莨菪碱的线性范围为(2.5-60μg/mL),4-氨基安替比林的线性范围为(2.5-60μg/mL),线性回归 R(0.9999-0.9998)。双氯芬酸、氢溴酸东莨菪碱和 4-氨基安替比林的LLOQ(15、2.5、2.5μg/mL)、LQC(45、7.5、7.5μg/mL)、MQC(55、25、25μg/mL)和 HQC(60、50、50μg/mL)分别进行了测定。UV 检测在 220nm 处进行。该方法根据 ICH 指南以及 FDA 指南进行了验证,以确定生物分析基质中的两种药物,均证明了准确性和精密度。通过比较两种方法的结果,发现准确性和精密度无统计学差异(p=0.05)。通过两种不同的工具(分析生态尺度得分为 83,AGREE-分析绿色度度量方法得分为 0.83)进行绿色评估,证明该方法具有环保性。该方法可用于常规质量控制实验室工作、药物滥用筛查和赛马运动的清洁。