Analyses for the Future

Size: px

Start display at page:

Download "Analyses for the Future"

Gabriel Carter
6 years ago
Views:

1 Analyses for the Future Tony Moffat, University of London, Brunswick Square, London WC1N 1AX, UK FIP Congress, 2006, Salvador Bahia, Brazil, 30 th August 2006 We want to prove: The proprietary product was manufactured by the license holder, eg Viagra tablets were made by Pfizer. The product was manufactured by the license holder and it contained the right active at the right potency, eg Cox made the diazepam 5mg tablets and they contained 5 mg of diazepam. The generic product contained the right active at the right potency, eg erythromycin tablets 250 mg contained 250 mg of erythromycin.

2 WHY NIRS No sample preparation Quick and easy Non-destructive Analyses both active and excipients Qualitative and quantitative Fingerprints whole matrix Huge amount of information

Absorbance (Log10(1/R)) NIR Absorbance Spectra of Lipitor Tablets 0.8 10 mg 0.

3 Absorbance (Log10(1/R)) NIR Absorbance Spectra of Lipitor Tablets mg mg mg Wavelength/nm

4 SNV of Absorbance (Log10(1/R)) NIR SNV of Absorbance Spectra of Lipitor Tablets mg 20 mg 40 mg Wavelength/nm BESITRAN 50mg Tablets, Pfizer, Spain Sertraline hydrochloride Calcium hydrogen phosphate Hydroxypropylmethyl cellulose Magnesium stearate Microcrystalline cellulose Polyethylene glycol Polysorbate-80 Sodium starch gycollate Titanium dioxide Iron Oxide

5 BESITRAN 50mg Tablets, Pfizer, Spain Madrid Barcelona C of G Plots of four different manufacturers of 100mg allopurinol tablets ( nm) A B C D

Cialis 4 batches A 1 batch C 8 batches C Cialis List of Excipients Tablet core: Film coat: Lactose monohydrate Croscarmellose sodium Hydroxypropylcellulose Microcrystalline cellulose Sodium

6 Cialis 4 batches A 1 batch C 8 batches C Cialis List of Excipients Tablet core: Film coat: Lactose monohydrate Croscarmellose sodium Hydroxypropylcellulose Microcrystalline cellulose Sodium laurilsulfate Magnesium stearate Lactose monohydrate Hypromellose Triacetin Titanium dioxide (E171) Iron oxide yellow (E172) Talc Eli Lilly and Company Ltd, Cialis, Summary of Product Characteristics

7 Absorbance Absorbance Cialis Tablets by NIRS Blue: mean of 4 batches authentic tablets Brown: 1 batch counterfeit tablets Wavelength Wavelength Cialis by HPLC Standards Counterfeit Cialis

Absorbance Absorbance Viagra 7 batches A 1 batch C 14 batches C Viagra Tablets by NIRS Blue: mean 7 batches authentic tablets Brown: 1 batch counterfeit tablets 0.6507 0.0262 0.5860 0.0202 0.5213 0.

8 Absorbance Absorbance Viagra 7 batches A 1 batch C 14 batches C Viagra Tablets by NIRS Blue: mean 7 batches authentic tablets Brown: 1 batch counterfeit tablets Wavelength Wavelength

9 Absorbance Absorbance Levitra Tablets by NIRS Blue: mean of 3 batches authentic tablets Brown: 1 batch counterfeit tablets Wavelength Wavelength Correlation in Wavelength Space Preparation Authentic Counterfeit Cialis Levitra Viagra

spf (17,22) 0.25 10 0.2 0.15 20 0.1 0.05 30 0 40-0.05-0.

10 Scaled Data Pixels Four component mix 0.3 suc_fru_xyl_ace_(mixr2)_30apt_1s_raw_abs_nrm.spf (17,22) Wavenumber (cm-1) Pixels

11 Pixels Pixels Pixels Pixels Pixels Viagra Tablets Spectra correlated with Sildenafil Pixels Pixels Pixels Pixels Pixels Stylised particle size differences of an active in two different manufacturer s tablets

12 Paracetamol Tablets 500 mg Sterwin Zanza Boots Excipients EXCIPIENT A B Br G S St T Z Magnesium stearate X X X X Maize starch X X X X X Methyl-p-hydroxybenzoate X Povidone X X X Propyl-p-hydroxybenzoate X Silicone dioxide X Sodium starch glycolate X X Stearic acid X X Talc X X X

14 Calibration and Validation Graphs (% m/m) Calibration Plot Validation Plot Results of Powders and Single Tablet Analyses (NIR Predicted % Paracetamol Label Claim) Mean Range Powders, RCA Intact Tablets, RCA Intact Tablets,Probe

15 Analytical Spectral Devices FieldSpec 3 (wireless) Laser 2000 EPP2000 NIR InGaAs Spectrometer

16 Identifyer Ahura Coprporation Acknowledgements Dr Roger Jee Dr Andrew O Neil Mr Yat Hang Mark Shek Dr Myoung-Hee Shin Dr Nicola Wilson

17 RPSGB Popular Products Popular Products

18 Pharmaceutical Journal 4 February 2006

19 Lustral 50 mg Madrid & Barcelona BESITRAN - 2nd PCA LOADING 2 nd component loadings Hydroxypropylmethylcellulose

20 Absorbance Absorbance Authentic Cialis (blue), Levitra (brown) and Viagra (green) Tablets and Pure Drugs Sildenafil Citrate Tadalafil Authentic Cialis Tablets Wavelength Wavelength nm Cialis PCA

21 Levitra Standards Counterfeit Levitra Centre of Gravity Plot (95% equal frequency ellipses)

22 Comparison between Samples Good sample Sticking sample

Etat des travaux du GDP

Etat des travaux du GDP (Avril 2018) Item General methods relevant to Q6A Dissolution (rev. 3) 4 Disintegration (rev. 1) 4 Uniformity of content/mass (rev. 2, corr. 1) 4 Tests for specified microorganisms