Validation and Development of a Method for Identification and Stability Analysis of Delafloxacin Separation Using LC-MS/MS

被引:0
作者
Sarbudeen, M. [1 ]
Abbaraju, V. D. N. Kumar [2 ]
Padmalatha, K. [3 ]
Kodali, Unati Sai [4 ]
Chinnamaneni, Satya Vani [5 ]
Mandava, Bhuvantej [6 ]
Rao, Mandava Venkata Basaveswarao [2 ]
机构
[1] Krishna Univ, Dept Chem, Machilipatnam 521004, Andhra Pradesh, India
[2] GITAM Univ, Dept Environm Sci, Visakhapatnam 521108, Andhra Pradesh, India
[3] Vijaya Inst Pharmaceut Sci Women, Vijayawada 521108, India
[4] Dr NTR Univ Hlth Sci, Dr Pinnamaneni Siddhartha Inst Med Sci & Res Fdn, Vijayawada, Andhra Pradesh, India
[5] Waters Corp, Principal QC Lab Tech, Milford, MA USA
[6] Sacred Heart Univ, Dept Healthcare informat, 5151 Pk Ave, Fair Fields, CT 06825 USA
关键词
LC-MS/MS; Validation; Linearity; Nano gram; MRM ion modeDelafloxacin; PLASMA;
D O I
10.13005/ojc/400112
中图分类号
Q5 [生物化学]; Q7 [分子生物学];
学科分类号
071010 ; 081704 ;
摘要
In order todevelop and validate the technique for delafloxacin authors are used the peak intense which is furthermore improved to this present investigation employing a variety of parameters, which includes column, alteration of eluent ratio, and rate of flow. For this development authors are usedWaters column with 2.1mmx100mm, 5 mu m, C18. Mobile phase as 0.2% formic acid with pH of 2.6 and acetonitrile in the proportion of 30v/v:70v/v. The retention was 1.2 min and the rate of flow is identified as 0.12 mu L/minute. Forced degradation studies reveals that the peaksobtained are homogeneousand there are noco-elutingpeaks. The %RSD was found to be 3.5. Six LLOQ concentrations (10 ng/ml-1)of delafloxacin were evaluated in order to carry out the precision study. The results of calibration curve were 232.8, 0.9968, and 1273, respectivelyfor slope, coefficient of correlation (r2), and intercept.Mass spectrum development is done by the utilization of MRM ion mode (ES+) with mass transitions of m/z 441.10>379.10 (amu). On ionization,both parent and daughter ions were identified. 10-150 ng/mL is the calibration curve which reveals that linear by lower quantification limit of 10.00 ng/mL. LOQ- 50.00 ng/mL, MOQ-100.00 ng/mL, HOQ-150.00 ng/mL set to accuracy studies.In this present study, the research could be very helpful inlocating other potential DPs and process -related impurities that might be present indelafloxacin in very small amounts.
引用
收藏
页码:95 / 101
页数:7
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