A quality-by-design evaluated liquid chromatography method development and validation for the separation and quantification of nitroxoline and its impurities.

A novel, isocratic, sensitive, stability-indicating high-performance liquid chromatography method was developed for the separation and quantification of related substances in nitroxoline (NTL). The chromatographic separation has been achieved on Inertsil ODS-3 V, (250 × 4.6 mm, 5 µm) at 240 nm using ethylenediamine tetraacetic acid buffer and methanol in the ratio of 60:40 v/v as mobile phase. The performance of the method has been checked as per the International Conference on Harmonization guidelines for specificity, linearity, accuracy, precision, and robustness. Regression analysis showed a correlation coefficient value greater than 0.99 for NTL and its three impurities. The detection limit of impurities was in the range of 0.01% (0.05 µg/mL)-0.22% (1.1 µg/mL) indicating the sensitivity of the newly developed method. The accuracy of the method was established based on the recovery obtained between 94.7% and 104.1% for all the impurities. The percentage relative standard deviation obtained for the repeatability was less than 4.0% at the specification level for all impurities. Forced degradation was performed to establish the stability-indicating nature of the method and to know about the degradation products, the quality of a drug substance changes with time under the influence of stress conditions. Thus, the proposed method was validated and found to be specific, sensitive, linear, accurate, precise, reproducible, and beneficial for routine usage.

Association of TNFSF11 rs2200287 and TNFSF11 rs2148072 gene polymorphisms in preeclampsia.

BACKGROUND: Various cytokines released by white blood cells like lymphocytes are linked to the immune system during pregnancy. The polymorphism of the TNFSF11 (rs2200287 and rs2148072) gene is related to the preeclampsia of pregnancy. MATERIALS AND METHODS: This study was a prospective study involving 304 pregnant women with preeclampsia (n = 152) and controls (non-preeclamptic pregnant women) (n = 152). To investigate the rs2200287 and rs2148072 SNP's of TNFSF11 gene polymorphism by using the PCR-RFLP techniques. RESULTS: A significantly different genotype distribution of TNFSF11 (rs2200287 and rs2148072) polymorphisms were observed between the two groups, with the G allele of variant rs2200287 was highly significant in the preeclamptic group (P = 0.000; .5814; OR = .5814; 95% CI = .4211-.8012). And the C allele of variant rs2148072 was also highly significant in the preeclamptic group (P = 0.000; OR = .5076; 95% CI, .362-.71) in this study. CONCLUSION: The outcomes of the present study indicate that there was an association in TNFSF 11 (rs2200287 and rs2148072) gene polymorphism with preeclampsia compared to non-preeclampsia women.