Ultra Performance LC with Photo Diode Array Detection for the Development of Methods: Impurity Profiling and Long Term Stability Studies

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1 Ultra Performance LC with Photo Diode Array Detection for the Development of Methods: Impurity Profiling and Long Term Stability Studies Pittsburgh Conference Orlando, FL 14MAR06

2 Observations The pressure on pharmaceutical scientists to produce larger quantities of relevant information increases daily Bottlenecks in the process are often technology-based Advances in technology drive growth Cost to bring a new Drug to Market? $1.2B Million Time to bring a new Drug to Market? 12 Years $1.9 Million per Week $48,000 per Hour Value of Generics 180 Day Exclusivity in North America? Establishes Market Dominance Helps Solidify long term Market Share

3 LC Technology Landscape s 70 s 80 s 90 s 00 s Increasing Refinement & Consistency 1959 GPC - Dow Columns & Waters instrumentation 1967 Waters 1st LC 1968 FAB MS Data advances M6000 CE introduced from integrators 1993HPLC Pump to computers First relational 1973 DB CDS µbondapak C18 - Turbochrom Millennium Maxima Sep-Pak s HP 1100 SFC introduced WISP Alliance Advances in 1999 XTerra laboratory networking 2000 ZQ Mass Detector AutoPurification 2002 IS Columns Atlantis Empower CapLC 2003 Quattro Premier LCT Premier

4 Instrument Modification Working at the limits of HPLC Typical modifications and adaptations (and sources of variability) System volumes Gradient mixing Injector volumes and loop sizes Detector cells Particle size MS inlet considerations Software controls (inject delay, gradient delay) Column dimensions To meet these challenges many laboratories use HPLC at the extremes of its capabilities

5 Intelligent Speed Technology When you just need Speed Introduced and launched in 2002 Waters developed 20 mm length Intelligent Speed (IS ) columns in 2.1, 3.0, 3.9 and 4.6 mm ID s Used for scaling down separations originally run on long columns (i.e., 150 mm length) Developing new separations / Method Development Time savings

6 Objective: to perform fast chromatography with HPLC instrumentation Instrument Modification Working at the limits of HPLC 5μm C18 HPLC System Modifications: IS Column Reduced system volume (injector) Software controls, inject delay Rs= Tricyclic Antidepressants 1. Nordoxepin 2. Desipramine 3. Nortriptyline 4. Doxepine 5. Imipramine 6. Desipramine 7. Trimipramine Resolution challenge = misinformation, lost information = unreliable integration, lost time = quality of data is compromised

7 Instrument Modification Working at the limits of HPLC 5μm C18 HPLC μbore flow cell System Modifications: Reduced system volume (injector) Software controls, inject delay Utilization of μbore flow cell Rs= Tricyclic Antidepressants 1. Nordoxepin 2. Desipramine 3. Nortriptyline 4. Doxepine 5. Imipramine 6. Desipramine 7. Trimipramine Improvement in Resolution (1.4 to 1.8) 2.4X loss in sensitivity 7 Sensitivity challenge = unreliable integration = lost information

8 ACQUITY UPLC TM The best approach to chromatography 1.7μm UPLC 1 No Modification: ACQUITY System 2 3 Rs= Tricyclic Antidepressants 1. Nordoxepin 2. Desipramine 3. Nortriptyline 4. Doxepine 5. Imipramine 6. Desipramine 7. Trimipramine 1.8 improvement in resolution 1.7X increase in sensitivity No Compromise: Resolution, speed and sensitivity

9 The challenge of the van Deemter plot Van Deemter Plots Influence of Particle Size Particles are central to the quality of the separation Smaller particles provide increased efficiency With smaller particles this efficiency increase extends over a wider linear velocity This provides the ability for both added resolution and increased speed of separation All particles eventually loose efficiency to linear velocity

10 UPLC Separations A new category of liquid chromatography

11 Small Particles with Traditional HPLC Working at the limits of HPLC Metabolites of Caffeine on HPLC XTerra MS C x 50 mm, 2.5 µm F = 0.5 ml/min PSI MAX = 3,950 T (4) = 1.30 N (4) = 4,100 Rs (2,3) = ACQUITY UPLC BEH C x 50 mm, 1.7 µm F = 0.3 ml/min PSI MAX = 4,200 T (4) = 1.63 N (4) = 5,400 Rs (2,3) = AU AU Minutes Minutes

12 Fundamental Resolution Equation At Constant Column Length Rs = N 4 ( α -1 α ) ( k ) k+1 System Selectivity Retentivity Efficiency In UPLC systems, N (efficiency) is the primary driver Selectivity and retentivity are the same as in HPLC Resolution, Rs, is proportional to the square root of N Rs And, Efficiency (N), is inversely proportional to Particle Size, dp So: N N 1 dp Therefore: dp 3X, N 3X, Rs 1.7X

13 Flow Rate & Back Pressure At Constant Column Length Back Pressure is proportional to Flow Rate, F, and inversely proportional to Particle Size squared ΔP FR 1 dp Optimal Flow Rate is inversely proportional to Particle Size 1 F opt dp 2 dp 3X, P 27X

14 Optimal Linear Velocity on ACQUITY UPLC Metabolites of Caffeine HPLC Non-Optimal Linear Velocity UPLC Optimal Linear Velocity AU ACQUITY UPLC TM BEH C x 50 mm, 1.7 µm HPLC F = 0.3 ml/min PSI MAX = 4,200 T (4) = 1.63 N (4) = 5,400 Rs (2,3) = 0.97 AU ACQUITY UPLC TM BEH C x 50 mm, 1.7 µm ACQUITY UPLC TM F = 0.6 ml/min PSI MAX = 8,400 T (4) = 1.02 N (4) = 10,100 Rs (2,3) = Minutes Minutes

15 New 2 nd Generation Hybrid ACQUITY UPLC Chemistry Improved Strength Improved Efficiencies Improved Peak Shape Wider ph Range EtO EtO Si Si CH 2 CH 2 Si O O O Si OEt OEt O O Si Si Polyethoxysilane (BPEOS) OEt O OEt O O Et Et n 4 EtO Si EtO EtO OEt Tetraethoxysilane (TEOS) + EtO EtO Si EtO CH 2 CH 2 OEt Si OEt OEt Bis(triethoxysilyl)ethane (BTEE)

16 ACQUITY UPLC Column Chemistries C18 C8 Trifunctionally Bonded C 18 Proprietary Endcapping Widest ph range Trifunctionally Bonded C 8 Proprietary Endcapping Widest ph range Shield RP18 Monofunctionally bonded Embedded polar group Phenyl Trifunctionally Bonded C 6 Phenyl Proprietary Endcapping

17 ACQUITY UPLC Reversed-Phase Column Selectivity Chart 3.6 Waters Spherisorb S5 P (ln [α] amitriptyline/acenaphthene) Waters Spherisorb S5CN Nova-Pak CN HP Hypersil CPS Cyano Hypersil BDS Phenyl YMC-Pack CN Inertsil CN-3 Inertsil Ph-3 Hypersil Phenyl YMC-Pack Phenyl Nova-Pak Phenyl YMC J'sphere ODS M80 YMCbasic Chromolith Nova-Pak YMC J'sphere ODS H80 XTerra TM RP-18 C18 Phenyl Nova-Pak Luna YMC-Pack ODS AQ YMC-Pack Pro C4 C8 Phenyl Hexyl Atlantis dc18 YMC-Pack Pro C8 YMC-Pack ODS-A ACT Ace C18 Symmetry C8 Zorbax XDB C18 XTerra Luna MS C8 YMC-Pack Inertsil ODS-3 C8 (2) Pro C18 SunFire C18 XTerra Luna SunFire C8 MS C18 C18 Symmetry C18 SymmetryShield RP8 (2) XTerra RP18 Zorbax SB C18 SymmetryShield RP18 XTerra RP8 YMC-Pack PolymerC18 (ln [k] acenaphthene) YMC J'sphere ODS L80 µbondapak C18 Waters Spherisorb ODS1 Resolve C18 Waters Spherisorb ODS2 Nucleosil C

18 EXPANDED VIEW Chromolith TM RP-18 The Modern C 18 Zone Selectivity Chart Nucleosil C18 (ln [α] amitriptyline/acenaphthene) Zorbax Rx C18 Zorbax Eclipse XDB C18 YMC-Pack Pro C18 Luna C18 Inertsil ODS-3 XTerra Kromasil C18 MS C18 Luna C18(2) Zorbax Extend C18 Prodigy C18 Hypersil HyPurity Elite C18 Inertsil ODS-2 Hypersil Elite C18 Supelcosil LC-ABZ+Plus Atlantis dc18 XTerra RP18 Supelcosil LC DB-C18 YMC-Pack ODS AQ Polaris C18-A Symmetry C18 SymmetryShield RP (ln [k] acenaphthene)

19 The Modern C 18 Zone ACQUITY UPLC BEH Chemistry EXPANDED VIEW Nucleosil C Chromolith TM RP-18 (ln [α] amitriptyline/acenaphthene) ACQUITY UPLC BEH C8 Atlantis dc18 Zorbax Rx C18 Zorbax Eclipse XDB C18 ACQUITY YMC-Pack Pro UPLC C18 BEH Luna Phenyl C18 Inertsil ODS-3 Kromasil C18 XTerra MS C18 Luna C18(2) Zorbax Extend C18 Prodigy C18 Hypersil HyPurity Elite C18 Inertsil ODS-2 Hypersil Elite C18 Supelcosil LC-ABZ+Plus XTerra RP18 Supelcosil LC DB-C18 YMC-Pack ODS AQ ACQUITY UPLC Symmetry BEH C18 C18 Polaris C18-A ACQUITY UPLC BEH Shield RP18 SymmetryShield RP (ln [k] acenaphthene)

20 UPLC Separations How can we realize the potential?

21 UPLC Technology Challenges Realizing the potential Holistic design High pressure fluidic modules Low system volume High speed detectors; optical and mass Low dispersion detector cell New module communication protocols Reduced cycle time autosampler Minimum carryover Controlled and coordinated interaction Software designed for system integration Comprehensive diagnostic suite

22 UPLC Technology Challenges Ultra Performance by Design Holistic design System Considerations: Small Footprint Rugged and reliable Redesigned and optimized fluidics Consolidated waste management Integrated system diagnostics Connections Insight remote diagnostics

23 UPLC Technology Challenges Ultra Performance by Design Holistic design Binary Solvent Manager: High pressure blending Binary gradients Four solvent reservoirs On-line degassing Low dispersion design UPLC pressure capabilities

24 ACQUITY UPLC Binary Solvent Manager gradient steps N = 6 1% Steps 0% B to 10% B Flow Rate=0.50 ml/minute Backpressure ~9300 psi

25 ACQUITY UPLC Binary Solvent Manager AutoBlend 5.0% ACN 4.0% ACN Injections of Caffeine with AutoBlend at 1.0mL/min 4.0% to 5.0% ACN in 0.1% Increments

26 UPLC Technology Challenges Ultra Performance by Design Holistic design Sample Manager: Low dispersion XYZZ Format Variable volume fixed loop injector Low volume injections Fast cycle times Dual solvent needle wash Low carryover Plates and/or vials 96 Vials 2 Plates, 96 or 384 well format (192 to 768 samples) Thermal control (4-40 o C) Pressure optimized fluidics

27 ACQUITY UPLC Sample Manager Performance - Linearity Area R 2 = Amount 0.1 mg/ml Acetaminophen with 20µL loop

28 ACQUITY UPLC Sample Manager Performance -Carryover 10mg/mL Human Insulin Carryover %

29 UPLC Technology Challenges Ultra Performance by Design Holistic design Sample Organizer: (optional) Expands capacity 22 Shallow Well Plates Up to 8,448 Samples 15 Deep Well Plates 8 Vial Plates Shuttles plate feed Thermal control (4-40 o C)

30 ACQUITY UPLC Column Manager with ecord Holistic design Column Manager: Innovative pivot design Positions column to detector Up to 65 o C ecord connection Paperless tracking of column manufacturing and history Nonvolatile read/write memory Fixed column manufacturing data Unique column identification Certificate of Analysis QC test data Variable column usage data Column use data Gathered through life of column ecord Reader Microchip

31 ecord Technology Column manufacturing information Paperless Certificate of Analysis & Performance Chromatogram Data (information can be printed if desired)

32 ecord Technology Column history file

33 UPLC Technology Challenges Ultra Performance by Design Holistic design Detectors: Optical, ELSD, and/or Mass Spectrometers Tunable UV or Photodiode Array Optimized and proprietary flow cell for UPLC High speed data sampling

34 ACQUITY UPLC Optical Flow Cell Design Light Guided UPLC flow cells 10 mm pathlength, 500 nl volume Flow cell channel is the inside of a low-index Teflon AF tube Total internal reflection at walls, like optical fiber cladding α water Teflon AF Teflon AF d

35 ACQUITY UPLC Software Control Required features incorporated in current software Empower MassLynx More information System monitoring Performance history ecord column tracking Easy to use Graphically oriented Reduce training and re-acquainting

36 ACQUITY UPLC Console Access to status and control

37 ACQUITY UPLC Console Access to status and control

38 UPLC Examples Method Conversion Convert an existing HPLC method to ACQUITY UPLC Objectives Need faster analysis for sample throughput Need resolution to quantify Result Method was successfully converted with sample injection cycle times reduced from 10 minutes to <2 minutes Resolution was maintained for quantitative purposes

39 8 Diuretics + impurity ACQUITY UPLC Transfer: HPLC to HPLC Rs = 2.30 Rs = 1.86 Vendor A HPLC 2.1x100mm 5µ C Rs = 6.45 Rs = 3.01 ACQUITY System (HPLC) 2.1x100mm 5µ C18 Time in Minutes

40 8 Diuretics + impurity ACQUITY UPLC Transfer: HPLC to UPLC 0.30 AUFS Rs = 1.86 Rs = x100mm 5.0µm C18 Vendor A HPLC 0.30 AUFS Rs = 4.71 Rs = x100mm 1.7µm ACQUITY BEH UPLC C18 More Resolution ACQUITY UPLC Time in Minutes

41 8 Diuretics + impurity HPLC and UPLC Applying the UPLC theory: L/dp 0.30 Rs = x100mm 1.7µm ACQUITY UPLC AUFS Rs = 4.71 ACQUITY UPLC 0.33 AUFS x30mm 1.7µm ACQUITY UPLC Shorter column = Scaled Gradient Same Resolution as HPLC, Less Time ACQUITY UPLC Time (min)

42 HPLC and UPLC Applying the theory: Final assay 0.33 AUFS 8 Diuretics + impurity 2.1x30mm 1.7µm ACQUITY UPLC Scaled Gradient Same Resolution as HPLC, Less Time ACQUITY UPLC 0.25 AUFS Time (min) AUFS 2.1x30mm 1.7µm ACQUITY UPLC Scaled gradient, optimized flow rate Same Resolution as HPLC Much Less Time (6.25 X) Rs = Time Time (min) 1.6

43 ACQUITY UPLC Calculator making method development easy

44 UPLC Examples Method Development Different from HPLC Method Development? An extension of everything you already know from HPLC Can we take advantage of the ACQUITY UPLC Systems: Theoretical Speed advantage? Theoretical Sensitivity advantage? Theoretical Resolution advantage? Generic Gradient? Sample dependent, but Starting with a 4 minute and a 8 minute 0% to 100% Organic linear gradient will typically generate enough data to calibrate the separation.

45 Related Compound Analysis Method Development process for 7 related compounds (coumarins) Analytical considerations Speed, 60 second separation? Resolution, meet USP requirements Reproducibility Robustness Sensitivity Method development in less than: A week? A day? A morning or afternoon? An hour?

46 Initial Generic Shallow Gradient 0%-100%B, 8 minutes, 0.8mL/min 0 9 minutes % 0.45 AU % Minutes

47 Initial Generic Intermediate Gradient 0%-100%B, 4 minutes, 0.8mL/min minutes 100% 0.54 AU % Minutes

48 10%-60%B, 2 minutes, 0.8mL/min 0 17 minutes AU Minutes

49 10%-80%B, 2 minutes, 0.8mL/min 0 20 minutes AU Minutes

50 10%-80%B, 1.5 minutes, 1.0mL/min 0 22 minutes AU Minutes

51 5%-80%B, 1.5 minutes, 1.0mL/min, Curve minutes AU Minutes

52 5%-80%B, 1.0 minute, 1.0mL/min, Curve minutes AU Minutes

53 ACQUITY UPLC PDA Building libraries for peak tracking nm nm nm nm nm nm nm

54 Coumarin standards overlay AU Hydroxycoumarin glucunoride Hydroxycoumarin AU Hydroxycoumarin AU AU 0.00 Coumarin Methoxycoumarin AU 0.00 AU Ethoxycoumarin Ethoxycoumarin AU Minutes

55 Coumarin standards overlay Composite Chromatogram minutes AU Peaks 7-Hydroxycoumarin - gluconoride 7-Hydroxycoumarin 4-Hydroxycoumarin Coumarin 7-Methoxycoumarin 7-Ethoxycoumarin 4-Ethoxycoumarin Minutes

56 5%-80%B, 1.0 minute, 1.0mL/min, Curve minutes AU Peaks 1. 7-Hydroxycoumarin - gluconoride 2. 7-Hydroxycoumarin 3. 4-Hydroxycoumarin 4. Coumarin 5. 7-Methoxycoumarin 6. 7-Ethoxycoumarin 7. 4-Ethoxycoumarin Minutes

57 5%-80%B, 1.0 minute, 1.0mL/min, Curve 4 1 RT Area % Area Height Selectivity USP Resolution USP Tailing 1.02 K Prime AU Minutes

58 Review UPLC Method Development Method Development process for 7 related compounds (coumarins) Completed = = Analytical considerations Speed, 60 second separation? Resolution, meet USP requirements Reproducibility Robustness Sensitivity Completed = = Method development in less than: A week? A day? A morning or afternoon? An hour? Completed in 48 mins = =

59 Challenges in Qualitative Analysis Complexity of the Task Detection of all the analytes of interest in the sample Resolution of isomers and closely related analytes Resolution of analytes of interest from endogenous components in the sample Improving throughput Analyte detection in LC depends upon a high quality LC separation Options LC resolution can be improved by increasing column length or reducing particle size Column efficiency increases with the square root of the column length Small particles give increased performance with reduced analysis time Increased column length results in longer analysis times

60 Impurity Definitions What is an impurity: An entity of the drug substance or drug product that is not the chemical entity defined as the drug substance, an exipient, or other additives to to the drug product. Degradation product (ICH): A molecule resulting from a change in the drug substance (bulk material) brought about over time. For the purpose of stability testing of the products in this guidance, such changes could occur as a result of processing or storage (e.g. deamidation, oxidation, aggregation and proteolysis). In the pharmaceutical industry, an impurity is generally considered as any other organic material besides the drug substance or active pharmaceutical ingredient. Ref. Handbook of Isolation and Characterization of Impurities in Pharmaceuticals. Edited by Satinder Ahuja and Karen Mills Alsante.

61 Impurity Common Names Classes of impurities are inorganic, organic, biochemical, polymeric Sources of impurities Intermediates/penultimate intermediate Transformation products, intermoleculer interaction, rearrangements Degradation (hydrolysis/oxidation) Related products: compounds produced with a similar structure (these sound less dangerous, but can be lethal in small quantities, due to similar activity structure) By products: unplanned compounds produced by synthesis Enantiomers

62 UPLC for Impurity Profiling Ranitidine HCl O - H N + O 3 C CH 3 N O NH S HN CH 3 Ranitidine [M+H] = (active) N O OH {5-[(dimethylamino)methyl]-2-furyl}methanol [M+H] = (D) H 3 C adduct [M+H] = (J) N C H 3 CH 3 N O CH 3 O S S O O - N + NH NH NH NH H 3 C H 3 C N + O - O N HN S H 3 C CH 3 N N CH 3 OH R - one oxime [M+H] = (A) CH 3 H 3 C N O S O O - S - oxide [M+H] = (C) NH N + O NH CH 3 O - H N + O 3 C CH 3 N O NH S HN CH 3 R-nitroacetamide [M+H] = (E) O NH 2 S R - ethanamine [M+H] = (F) H 3 C CH 3 N H 3 C CH 3 N O O S O - NH N + NH CH 3 O S NH O N + O - N - oxide [M+H] = (Note: covalent bonded Oxygen) O N,N bis [M+H] =

63 Ranitidine HPLC current HPLC method A Conditions Column: XTerra MS C18 Dimensions: 150 x 3.9mm, 5μm Mobile Phase A: 20mM Amm. Bicarbonate ph 9.0 Mobile Phase B: Methanol Flow Rate: 1.5 ml/min Gradient: Time Profile (min) %A %B Injection Volume: 5.0 μl Temperature: 500C Detection: 230 nm G - Active J AU B D C E F H I *K Minutes

64 Final UPLC Method analysis time reduced by a factor of Conditions A G - Active C J AU Column: Waters ACQUITY UPLC BEH C18 Dimensions: 100 x 2.1mm, 1.7μm Mobile Phase A: 20mM Ammonium Bicarbonate Mobile Phase B: Methanol 300uL Flow Rate: 0.45 ml/min Gradient: Time Profile (min) %A %B Injection Volume: 1.0 μl Temperature: 50 C Detection: 230 nm B I F D H E *K Minutes

65 HPLC Separation of Terbinafine Rs = 2.37 C x 150 mm, 5 µm F = 300 µl/min 214 nm 5 Terbinafine

66 UPLC Degradation Analysis of Terbinafine Choices available: Increased speed and sensitivity with the same resolution Increased resolution and sensitivity at the same speed Speed Resolution Sensitivity

67 Improved Throughput and Sensitivity: Stability-Indicating Assays Rs = x 150 mm, 5 µm C 18 F = 300 µl/min 214 nm Height (µv) Deg 5 = 6,136 5 Terbinafine (F 2X, L 3X) Speed 6X Rs = Terbinafine 9 ACQUITY UPLC TM BEH C x 50 mm, 1.7 µm F = 600 µl/ min 214 nm Height (µv) Deg. 5 = 15,656 Sensitivity 2.5X Rs = 1X AU Minutes

68 Improved Resolution and Sensitivity: 100 mm, 1.7 µm column Rs = x 150 mm, 5 µm C 18 F = 300 µl/min 214 nm Height (µv) Deg 5 = 6,136 5 Terbinafine Speed = 1X Sensitivity 2X au Rs = Terbinafine ACQUITY UPLC TM BEH C x 100 mm, 1.7 µm 9 F = 500 µl/min 214 nm Height (µv) Deg 5 =12,572 65% ACN Rs = 1.8X Minutes

69 Conclusions Benefits of applying UPLC to stability-indicating assays: Develop faster and more sensitive assays while maintaining existing resolution (2.1 mm i.d.) Speed 6X Sensitivity 2.5X Develop sensitive, higher resolution assays within the same analysis time (100 mm length) Rs = 1.8X Sensitivity 2X

70 Conclusions UPLC generated significantly improved chromatography Increased resolution reduces analyte co-elution Enhanced resolution of UPLC significantly increases throughput and sensitivity With UPLC analytes are resolved that before remained undetected

71

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