Chemometric-assisted determination of some bisphosphonates and their related substances in pharmaceutical forms by ion chromatography with inverse UV detection
Bibliographic record
Abstract
A simple ion chromatographic (IC) method was developed and validated for simultaneous or individual determination of zoledronic, alendronic, pamidronic acids and their related substances in pharmaceutical formulation. The analytes were separated on Waters IC-Pak Anion HR analytical column with a nitric acid (3 mM) without any other additives, as mobile phase at a flow rate of 1.0 mL min−1. Inverse UV detection was used at 240 nm. Important chromatographic factors that influence the chromatography responses were screened by 11/12 Pluckett–Burman design and their interaction were assayed by 23 full factorial design. The RP-HPLC method was optimized with the aid of LC-Simulator® (ACD Labs, Toronto, Ontario, Canada) software. Validated method was successfully used for quantitative analysis of PAMIFOS®, concentrate for infusion (Habitfarm AD, Ivanjica, Serbia), ZOMETA®, powder for infusion (Novartis Pharma, Stein AG, Switzerland) and BONAP® tablets (Hemofarm, Vrsac, Serbia). Total chromatographic analysis time per sample was approximately 6 min, which represents significant improvement over existing methods. Validation studies revealed that the method is specific, rapid, reliable, and reproducible. Calibration plots were linear over the concentration ranges 20–120 μg mL−1 and 0.1–2 μg mL−1 for bisphosponates and their related substances, respectively. The LODs were 8.7, 4.7, 2.5, 0.026 and 0.011 μg mL−1 for alendronate, pamidronate, zoledronate, phosphoric acid and phosphorous acid, respectively.
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How this classification was reachedexpand
Full frame distilled prediction
Teacher imitationNot calibrated prevalence, not ground truth. Human validation pending. Learned from the 10,348 direct Codex labels and 10,348 direct Gemma labels. Candidate is the union of thresholded teacher heads; consensus is their intersection. These outputs are machine_predicted_unvalidated and are not human labels or direct frontier model labels.
Codex and Gemma teacher scores by category
| Category | Codex | Gemma |
|---|---|---|
| Metaresearch | 0.000 | 0.000 |
| Meta-epidemiology (narrow) | 0.000 | 0.000 |
| Meta-epidemiology (broad) | 0.000 | 0.000 |
| Bibliometrics | 0.001 | 0.003 |
| Science and technology studies | 0.000 | 0.000 |
| Scholarly communication | 0.000 | 0.000 |
| Open science | 0.000 | 0.000 |
| Research integrity | 0.000 | 0.000 |
| Insufficient payload (model declined to judge) | 0.000 | 0.000 |
Machine scores (provisional)
The two teacher heads of the student model, read on this work. A score orders the frame for review; it never asserts a category, and the validation status ships verbatim with every row.
Baseline scores from an immature model (maturity gate not passed, 7 training rounds). Scores rank; they never assert a category.
score_only:v0-immature-baseline · verbatim from the scoring run: score_only means the number may rank works, and no category label ships from itClassification
machine, unvalidatedMachine predicted; a candidate call from one teacher head, not a consensus.
How this classification was reached, model by model and score by score, is at the end of the page under "How this classification was reached".