Eco-Friendly Direct GC–MS Method for Estimation of Niacin and Related Impurities Involving Pyridine in Food Supplements
Abstract
:1. Introduction
2. Experimental Analysis
2.1. Instruments
2.2. Materials and Reagents
2.2.1. Standards
2.2.2. Pharmaceutical Formulation
2.2.3. Chemicals and Solvents
2.3. Standard Solutions
2.3.1. Stock and Working Standard Solutions
2.3.2. Solutions of Pharmaceutical Formulation
2.4. Chromatographic Conditions
2.5. Calibration Curve Construction
2.6. Application to Pharmaceutical Formulation
3. Validation of the Newly Developed Method
3.1. Linearity
3.2. Accuracy
3.3. Precision
Repeatability
3.4. Intermediate Precision
3.5. Specificity
Limits of Detection and Quantitation (LOD and LOQ)
3.6. System Suitability
4. Results and Discussion
4.1. Method Development and Optimization
4.2. Results of Figures of Merit
4.3. Results of Assay of Dosage Form
4.4. Eco-Scale Assessment of Proposed Method
5. Conclusions
Supplementary Materials
Author Contributions
Funding
Institutional Review Board Statement
Informed Consent Statement
Data Availability Statement
Acknowledgments
Conflicts of Interest
Abbreviations
GC–MS | Gas chromatography–mass spectrometry |
ISO | isonicotinic acid |
MP | 5-ethyl-2-methylpyridine |
NIA | niacin |
PCD | pyridine-2, 5-dicarboxylic acid |
SIM | selected ion monitoring |
USP | United States pharmacopeia |
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Components of the Analyzed Mixture | Regression Equation * | Retention Time |
---|---|---|
NIA | A1 = 0. 9636 C1 + 0.5158 | 5.68 |
PYR | A2 = 36.61 C2 + 8.2884 | 1.67 |
MP | A3 = 10.15 C3 − 0.5745 | 3.57 |
PDC | A4 = 0.4934 C4 − 0.0726 | 7.00 |
ISO | A5 = 1.1665 C5 + 0.0874 | 7.76 |
GC–MS Method | Parameter | ||||
---|---|---|---|---|---|
ISO | PDC | MP | PYR | NIA | |
0.5–20 | 0.5–20 | 0.1–5 | 0.005–5 | 0.5–20 | Range (µg mL−1) |
1.1665 | 0.4934 | 10.1500 | 36.6100 | 0.9636 | Slope |
0.0874 | −0.0726 | −0.5745 | 8.2884 | 0.5158 | Intercept |
0.9999 | 0.9998 | 0.9999 | 0.9999 | 0.9997 | Regression coefficient |
101.03 ± 1.729 | 100.95 ± 2.100 | 100.17 ± 1.064 | 99.69 ± 1.607 | 100.49 ± 0.754 | Accuracy (Mean ± SD) |
2.074 | 1.305 | 1.719 | 1.613 | 1.513 | Precision
|
2.464 | 2.434 | 2.200 | 2.515 | 2.122 | |
0.139 | 0.136 | 0.030 | 0.001 | 0.121 | LOD (µg mL−1) |
0.460 | 0.450 | 0.098 | 0.003 | 0.400 | LOQ (µg mL−1) |
Recovery % b | Pure Found (µg mL−1) | Pure Added (µg mL−1) | Found% a Mean ± SD) | Claimed Taken (µg mL−1) | Niacin® Tablets, Batch No. 152405-05 |
---|---|---|---|---|---|
98.67 | 2.96 | 3.0 | 100.11 ± 1.755 | 5.0 | NIA |
99.60 | 4.98 | 5.0 | |||
99.33 | 9.93 | 10.0 | |||
99.20 ± 0.391 | Mean ± SD |
Reference Values [35] | GC/MS | Parameter | |||||||
---|---|---|---|---|---|---|---|---|---|
ISO | PDC | NIA | PDC | NIA | MP | PYR | MP | ||
~1 | 1.5 | 1.3 | 1 | 1.3 | 1 | 1.4 | 1.3 | 1.4 | Tailing factor (T) |
1–10 | 6.76 | 6 | 4.68 | 6 | 4.68 | 2.57 | 0.67 | 2.57 | Capacity factor (K’) |
Acceptable | |||||||||
Rs > 1.5 | 3.185 | 6.26 | 2.64 | 1.67 | Resolution (RS) | ||||
>1 | 3.84 | 1.82 | 1.28 | 1.13 | Selectivity(α) | ||||
Increase with efficiency of the separation | 214,285.71 | 35,714.29 | 11,718.75 | 35,714.29 | 11,718.75 | 7092.2 | 3348.2 | 7092.2 | Column efficiency (N) |
The smaller the value the higher the column efficiency | 0.014 | 0.084 | 0.256 | 0.084 | 0.256 | 0.423 | 0.896 | 0.423 | HETP = height equivalent to theoretical plate, (cm/plate) |
Parameter | Reported HPTLC Method [31] ** | GC/MS | Reported HPLC Method [21] *** | GC/MS |
---|---|---|---|---|
Mean | 99.82 | 100.11 | 99.74 | 100.11 |
SD | 1.673 | 1.922 | 0.965 | 1.922 |
Variance | 2.797 | 3.697 | 0.931 | 3.697 |
n | 6 | 6 | 6 | 6 |
Student’s t-test * (2.228) | 0.283 | 0.430 | ||
F-test * (5.050) | 1.322 | 3.970 |
Reagent/Instruments | Penalty Points | ||
---|---|---|---|
Reported HPLC Method [20] | Reported HPTLC Method [30] | Proposed GC–MS Method | |
Helium | - | - | 1 |
Ethylacetate | 4 | - | |
Ethanol | 2 | - | |
Methanol | 12 | - | - |
Triflouroacetic acid | 8 | - | - |
Ammonia solution | - | 2 | - |
Technique (Energy used) | 0 | 0 | 2 |
Occupational hazard | 0 | 0 | 0 |
Waste | 5 | 3 | 5 |
Total penalty points | Σ25 | Σ11 | Σ8 |
Analytical Eco-scale Total score | 75 | 89 | 92 |
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Almalki, A.H.; Naguib, I.A.; Abdallah, F.F. Eco-Friendly Direct GC–MS Method for Estimation of Niacin and Related Impurities Involving Pyridine in Food Supplements. Separations 2021, 8, 46. https://doi.org/10.3390/separations8040046
Almalki AH, Naguib IA, Abdallah FF. Eco-Friendly Direct GC–MS Method for Estimation of Niacin and Related Impurities Involving Pyridine in Food Supplements. Separations. 2021; 8(4):46. https://doi.org/10.3390/separations8040046
Chicago/Turabian StyleAlmalki, Atiah H., Ibrahim A. Naguib, and Fatma F. Abdallah. 2021. "Eco-Friendly Direct GC–MS Method for Estimation of Niacin and Related Impurities Involving Pyridine in Food Supplements" Separations 8, no. 4: 46. https://doi.org/10.3390/separations8040046