21 CHAPTER-2 Table of Contents Chapter 2. Literature Survey S.No. Name of the Sub-Title Page No. 2.1 Literature survey for simultaneous selected drugs by RP-HPLC 2.2 Literature survey for simultaneous selected Drugs By UV- Spectroscopy 22-27 28-32
22 2. LITERATURE SURVEY 2.1 LITERATURE SURVEY FOR SIMULTANEOUS ESTIMATION OF SELECTED DRUGS BY RP-HPLC 2.1.1 Literature Survey for Estimation of Metformin Hydrochloride and Sitagliptin by RP- HPLC Method Table-2.1.1. Literature survey of metformin hydrochloride and sitagliptin S. No 1 2. Work RP-HPLC for simultaneous metformin RP-HPLC for simultaneous metformin Chromatographic Conditions C8 100x4.6mm, 3µm FR-0.6ml/min C 18-250 x4mm,5µm 1ml/min Mobile phase composition Phosphate buffer: ACN: CH 3OH 35:45:20 Phosphate buffer: ACN 60:40 Sita 50-150 Met 50-150 Sita 2-12 Met 20-120 tr (min) Sita-3.06 Met-2.42 Sita- 2.8 Met- 2 Ref 34 35 3. RP-HPLC for metformin hydrochloride C 18-250 x4mm,5µm Phosphate buffer: ACN 55:45 Sita 2-12 Met 20-120 -- 36 4 RP- HPLC for metformin hydrochloride C 8-100x4.6mm,5 µm 1mL/min Methanol :ACN :Phosphate buffer 20:35:45 Sita 10-30 Met 100-400 Sita-4.9 Met-3.69 37 5 HPLC for metformin in formulated microspheres and tablet dosage form phenomenex C18 column ACN:phosphate buffer 65:35 0-25 2.3 38
23 6 Method development and validation of metformin hydrochloride by Rp-Hplc Inertsil -C18-250x4.6mm 1-Octane sulfonic acid: ACN (80:20 1-250 2.5 39 7 8 9 HPLC Method For the metformin RP-HPLC development and validation for sitagliptin in Human Plasma Bioanalytical development and validation of Sitagliptin Phosphate by Rp-Hplc Atlantis d C18, 250 4.6 mm; 5.0 μm column, 1.0 ml/min INTERSIL C18 column (150 mm 4.6 mm, 5μm) 1.0 ml/min Phenomenex C18 (250 x 4.6mm, 5μ) 0.5% v/v of) 6.8 using orthophosphoric acid 1.0 ml/min 1-Heptane sulphonic acid:acn 75: 25 21-170 3.1 40 ACN: methanol: buffer 2:3:5 25-125 4.2 41 Triethylamine: ACN 77:23 10-1000 6.1 42 Impression on the above s: The literature review on the earlier studies publicized that there are few analytical s using HPLC technique. Most of the s utilized acetonitrile and buffers as the mobile phases. In an attempt to practice green chemistry this study was planned so as to avoid the acetonitrile and also to make the cost effective. In the proposed, methanol: phosphate buffer (with the change in ph with o-phosphoric acid) was used as mobile phase. This separated the analytes with greater efficiency, good resolution and decreased tailing factor, thus making the more simple, economic, precise and reliable. The was validated as per ICH guidelines.
24 Present work Chromatographic Conditions Agilent C8 Column (25 x 4.6 mm, 5µ) F.R-1.0 Detection wave length 267nm Mobile phase composition Methanol: Water (40:60) Met 100-450 Sita 10-45 tr (min) Met 3.03 Sita 7.03 tf Met 1.5 Sita 1.25 2.1.2 Literature survey for Estimation of Simvastatin and Sitagliptin by RP- HPLC Method Table- 2.1.2. Literature survey of simvastatin and sitagliptin S.No. 1 2. 3. 4 5 Work RP-HPLC for the simultaneous Simvastatin RP-HPLC for the simultaneous Simvastatin Simvastatin Determination of Simvastatin in Bulk and Pharmaceutical Formulation by HPLC Development and Validation of Simvastatin by RP-HPLC Method Chromatographic Conditions C 18-250 x4mm,5µm 1ml/min C 18-250 x4mm,5µm 1ml/min C4-150x4mm,3 µm 0.9ml/min C18 column (150x4.6 mm, 2.7 μm hypersil C18 column (250x4.6mm I.D., particle size 5 μm) 1.0 Mobile phase composition ADOP: ACN 50:50 Buffer: ACN: CH 3OH 40:35:25 ACN: OPA 70:30 CH3OH:OPA (10:90) Di hydrogen phosphate sodium : ACN 40:60 Sita 50-250 Sim 10-50 (tr) Sita 8.1 Sim 5.4 Sita 50-500 Sim 20-200 ---- Sita 50-500 Sim 20-200 5.0 60.0 μg/ml 10-200 μg/ml Sita 1.5 Sim 6.2 3.106 min Ref 43 44 45 46 47
25 6 7 Analytical Method Development and Validation of Simvastatin Bulk Drug by RP- HPLC Development and validation of HPLC for determination of Simvastatin ODS- 3V, 150mm 4.6mm, 5μ C18 column 150 X4.6 mm, I.D., 2.7 μ ACN: Buffer 60:40 CH 3OH:OPA (10:90) 1-150 μg/ml - 48 5.0-60.0 3.106 49 8 Stability- Indicating LC-UV Method to Assay Sitagliptin Phosphate Phenomenex C18 column (150mm x 4.6mm I.D., 5μm) 0.8 ml/ min phosphate buffer: acetonitrile 60:40 25-75 3.7 50 Impression on the above s: The literature review on the old studies publicized that there are analytical s involving liquid chromatographic techniques. Most of the s used ADOP, acetonitrile and buffers as the mobile phases. In an effort to practice green chemistry this study was planned so as to avoid the ADOP, acetonitrile and also to make the cost effective. In the proposed, methanol: phosphate buffer (with the change in ph with o-phosphoric acid) was used as mobile phase. Analytes were separated with greater efficiency, good resolution and decreased tailing factor, thus making the more simple, economic, precise and reliable. The was validated as per ICH guidelines.
26 Present work Chromatographic Conditions Agilent C 8 Column (25 x 4.6 mm, 5µ) F.R-1.0 Detection Wave length-253nm Mobile phase composition Methanol : Water (25:75) Sita 20-120 Simv 2-44 (t R) (t F) Sita- 3.22min Simva- 15.76 min Sita-1 Simva-1.2 2.1.3. Literature Survey for Estimation of Diclofenac Potassium and Tizanidine Hydrochloride by Rp-Hplc S.No Table-2.1.3 Literature review of diclofenac potassium and tizanidine hydrochloride Mobile phase Chromatographic Work composition t R Conditions 1. RP-HPLC tizanidine, diclofenac and paracetamol 2. RP-HPLC diclofenac potassium andtizanidine hydrochloride 3. New for determination of diclofenac sodium by HPLC C18-250 x4mm,5µm C 18-250 x4mm,5µm C 8-15X4.5mm,5 µm Phosphate buffer : ACN 60:40 Phosphate buffer : ACN 45:55 Methanol:ACN: water 60:20:20 -- Dic 10-50 Tiz 0.2-1 0.25-0.4 Tiz 5 Dic 8.61 Par 3.43 Dic 8.78 Tiz 4.75 Dic 2.0 Ref 51 52 53 4 Stability indicating HPLC Hypersil CN column (150 mm 5.0 mm, 5 μm) HAS: Methanol:ACN 50:57:18 1-5 3.2 54
27 for determination of tizanidine 5 Validated LC for assay of tizanidine 1.0 ml/min C18 Intersil column ACN: phosphate buffer 60:40 0.2-5 4.21 55 Impression on the above s: The literature review on the past studies revealed that there are few analytical s involving liquid chromatographic technique based on HPLC. Most of the s utilized acetonitrile and buffers as the mobile phases. In an attempt to practice green chemistry this study was planned so as to avoid the acetonitrile and also to make the cost effective. In the proposed, methanol: phosphate buffer (with the change in ph with o-phosphoric acid) was used as mobile phase. All the s used C18 column for the simultaneous quantifications which consume more time for elution. In this study, C8 column was used so that analytes were separated with less retention times, greater efficiency, good resolution and decreased tailing factor, thus making the more simple, economic, precise and reliable. The proposed was validated as per ICH guidelines. Present work Chromatographic Conditions Qualisil C 8 column (250 x 4.6mm, 5µ) F.R-1mL/min Detection wavelength-235nm Mobile phase composition Methanol and Ortho phosphoric acid (40:60) Dic 10-50 Tiz 2-10 tr Dic 5.9 Tiz 2.1 tf Dic1.1 Tiz 1.4
28 2.2 LITERATURE SURVEY FOR SIMULTANEOUS ESTIMATION OF SELECTED DRUGS BY UV SPECTROSCOPY 2.2.1 Literature survey for metformin hydrochloride and sitagliptin by UV spectroscopy Table 2.2.1 Literature survey of metformin hydrochloride and sitagliptin S.No. 1 2. 3. 4 5 7 Work Estimation of metformin and sitagliptin by UV spectroscopy Estimation of metformin and sitagliptin by UV spectroscopy metformin and sitagliptin metformin and sitagliptin by UV spectroscopy UV Spectrophotom etric for the determination of metformin Forced degradation studies of metformin by using UV spectroscopy Estimation Method 1.Absorbance Maxima 2. AUC Multi component Mode of Analysis Absorbance maxima First order derivative Spectroscopy Using molar absorptivity value First order derivative Spectroscopy Solvent Distilled water Distilled water Distilled water 0.1N NaOH Distilled Water Met 2-12 Sita 25-225 Met 1-27 Sita 1-40 Met 2-10 Sita 20-60 Met 2-20 Sita 10-100 Λmax (nm) 1.Met 232 Sita 266 2. Met 222 Sita 279 Met 232 Sita 267 Met 231 Sita 267 Met 216 Sita 238.5 Ref. 56 57 58 59 Met 1-16 Met 233 60 CH3OH Met 1-10 Met 237 61 Impression on the above s: The literature review on the past studies revealed that there are few UV spectroscopic s for the metformin
29 hydrochloride and sitagliptin in single and in combined dosage forms. Most of them are tedious estimation s. Present work was aimed at solving simultaneous equations for the simultaneous the two drugs and distilled water was used as common solvent thus making the more economic, less time consuming and reliable than the existing s. The proposed was validated as per ICH guidelines. Present work Estimation Method Solvent Λmax (nm) equations Distilled water Met 10-50 Sita 20-80 Met 232 Sita 266
30 2.2.2 Literature Survey for Estimation of Sitagliptin and Simvastatin by UV Spectroscopy Table.2.2.2. Literature survey of simvastatin S.No 1 2 3. 4. 5 Work sita and Simva by UV Spectroscopy Spectrophotom etric for estimation of sita and Simva Q-absorbance ratio for estimation of sita and Simva sita and Simva by different analytical techniques Stability Indicating UV Method for the Estimation of Sitagliptin Estimation Method Simultaneou s equations First order Derivative Spectrophoto metry Q- absorbance ratio Method A Simultaneou s equation Method B First order Derivative Method C Q-abs ratio first order derivative Solvent CH3OH :Water 90:10 (% v/v) CH3OH CH3OH: Water 40:60 C 2H 5OH and Water (% v/v) CH3OH Sita 10-50 Simv 5-25 Sita 10-50 Simv 4-20 Sita 10-60 Simv 2-12 Sita 55-150 Simv 3-15 10-100 mg/ml λmax (nm) Sita 238 Simv 267 Sita 238 Simv 277 Sita 267 Simv 239 Sita 267 Simv 238 Sita 275 Simv 230 Sita 267 Iso abs point 250 Ref 62 63 64 65 267 66 6 UV for determination of Sitagliptin in bulk and in Formulation first order derivative CH3OH and water 10-60 267 67
31 Impression on the above s: The literature review on the past studies revealed that there are few UV spectroscopic s for the simvastatin in single and in combined dosage forms. Most of the s use tedious calculations and correction procedures. Present work was based upon solvent extraction of the two drugs and estimation by linear line equation thus making the so simple, reliable and precise. The proposed was validated as per ICH guidelines. Present work Estimation Method Solvent λmax (nm) Solvent extraction and estimation by Linear line equation Sitagliptin- 0.1N HCl Simvastatin- Methanol: Water (40:60) Sita 10 to 50 Simva 6 to 20 Sita 246 Simv 232 S.No 1 2 2.2.3 Literature survey for Estimation of Diclofenac potassium and Tizanidine hydrochloride by UV spectroscopy Table-2.2.3. Literature survey of diclofenac potassium and tizanidine hydrochloride Estimation λmax Work Solvent Method (nm) Spectroscopic s for simultaneous determination of diclofenac and tizanidine Spectroscopic for Method A Multi wave length technique Method B equations Method C Absorbance ratio Isoabsorptive point 2% Dimethyl formamide Diclo 0-50 Tiz 0-25 CH3OH Diclo 0.5-8 Tiz 1-12 Diclo 277 Tiz 320 Diclo 279 Tiz 229 Ref 68 69
32 3 determination of Diclofenac and tizanidine Spectrophotomet ric diclofenac and tizanidine Vierodt s CH3OH and water Diclo 2-34 Tiz 2-20 Diclo 274.6 Tiz 319.6 70 Impression on the above s: The literature review on the past studies revealed that there are few UV spectroscopic s for the Diclofenac potassium and tizanidine hydrochloride. Above s utilized dimethyl formamide and methanol as the solvents. In the proposed, distilled water was used as common solvent thus making the more cost effective. The proposed was validated as per ICH guidelines. Present work Estimation Method equations Solvent Distilled water Diclo 2-30 Tiz 4-20 λmax (nm) Diclo 240 Tiz 225