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Introducing the PL-ELS 2100 & PL-ELS 2100 Ice Evaporative Light Scattering Detector

Introducing the PL-ELS 2100 & PL-ELS 2100 Ice Evaporative Light Scattering Detector. First Impressions. Compact, modern design Flat top Small (200x450x415mm) Operation via control panel and simple keypad Column connection at front of detector

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Introducing the PL-ELS 2100 & PL-ELS 2100 Ice Evaporative Light Scattering Detector

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  1. Introducing the PL-ELS 2100 & PL-ELS 2100 Ice Evaporative Light Scattering Detector

  2. First Impressions • Compact, modern design • Flat top • Small (200x450x415mm) • Operation via control panel • and simple keypad • Column connection at front • of detector • One exhaust tube at rear, one liquid waste port at front PL-ELS 2100 PL-ELS 2100 Ice

  3. Simple Operation • Two modes of operation • STANDBY • Power on • LED off • Heaters off • Gas at minimum flow rate (1.2 SLM) • Gas shuts off after 15 minutes RUN • Power on • LED on • Temperatures and gas flow controlled to set values

  4. Eluent inlet Principles of Operation • The ELSD principle of operation employs three distinct stages : • Nebulisation • Evaporation • Detection Gas Light Source Liquid waste

  5. Nebulisation Inside the nebuliser chamber, the liquid flow from the column is mixed with an inert gas (normally nitrogen) to form a fine plume of solvent droplets. The temperature controlled nebuliser is designed to give a uniform droplet size. Nebuliser Range: ambient to 90°C

  6. Evaporation The eluent droplets pass through a narrow heated chamber where the eluent is removed by evaporation leaving a fine mist of analyte particles. The evaporator tube has an additional gas input to aid removal of the mobile phase PL-ELS 2100 Ice: 10-80°C PL-ELS 2100: 30-120°C

  7. PL-ELS 2100 Design Feature for Ambient Temperature Operation • Current ELS detectors have design features that allow low temperature operation with water. • An ELSD designed to operate at low temperature in water has to overcome two major problems • The length of drying time experienced at low temperatures for water, compared to higher temperatures • Saturation of the evaporation tube (i.e 100% relative humidity), which prevents further evaporation

  8. Evaporating Water at Ambient Temperature Consider, that a 20µm droplet of water takes ca. 2.5 times longer to dry at 30°C than at 50°C. So reducing droplet size will reduce the drying time: • A Water droplet of 10µm dries 4x faster at 30°C than a 20µm droplet. However, decreasing droplet size reduces the sensitivity of an ELSD

  9. Drying time of water droplets as a function of evaporator temperature 10µm droplet dries 4x faster than 20µm droplet @ 30°C

  10. Evaporating Water at Ambient Temperature By lowering the relative humidity (RH) within the evaporation tube, water can be evaporated at ambient temperature, without changing droplet size. The PL-ELS 2100 uses a stream of nitrogen gas during the evaporation step to lower the relative humidity Using this “evaporation gas” the PL-ELS 2100 can evaporate water at ambient temperature.

  11. Drying Time of Water Droplets as a function of Relative Humidity (RH) 20µm droplet dries 3x faster at 30% RH compared to 70% RH @ 30°C

  12. PL-ELS 2100 Ice Design Feature for Sub-Ambient Operation The PL-ELS 2100 Ice comprises an Integrated Cooled Evaporator in combination with the ‘evaporation gas’ technology to provide sub-ambient operation The ‘evaporation gas’ is increased to compensate for the increase in relative humidity at sub-ambient temperatures This approaches enables the PL-ELS 2100 Ice to operate as low as 10°C.

  13. PL-ELS 2100 Ice Design Feature for Sub-Ambient Operation Aqueous eluents can be removed at 15°C Organic solvents (e.g. THF) can be evaporated as low as 10°C The benefit of operating below room temperature provides maximum sensitivity for low-molecular weight semi-volatile compounds.

  14. PL-ELS 2100 Ice Design Feature for Sub-Ambient Operation • Integrated cooled evaporator provides rapid heating/cooling • 35°C to 10°C in 10 minutes • 15°C to 80°C in 11 minutes • Accurate temperature control of evaporator tube eliminates variations in semi-volatile response, due to ambient temperature variations

  15. Detection The analyte particles enter an optical chamber where they are irradiated by a light source. The incident beam is scattered by the particles and the intensity of scattered light is proportional to the concentration of the analyte

  16. Digital Signal Processing • PL-ELS 2100/2100 Ice are equipped with digital signal processing for greater flexibility: • PMT output or gain (1-10) • Amplifies signal output by set value • Smoothing (1-50) • Adjustable according to peak width • LED intensity (0-100) • Light source can be adjusted according to column loading (e.g prep LC)

  17. Advantages of Evaporative Light Scattering Detection • Universal: responds to all compounds in the mobile phase • Detects compounds that do not possess a UV chromophore (eg polymers, sugars)

  18. Advantages of Evaporative Light Scattering Detection: Pharmaceutical Mixture Detects all components in a single run Samples : 1. α-cyclodextrin 2. ß-cyclodextrin 3. Ibuprofen Column: Aquasil C18 5µm, 150x4.6mm Eluent A: Water Eluent B: Acetonitrile Gradient: 50-95% B in 5 mins Flow Rate: 1.0 ml/min Inj Vol: 20µl Detector: PL-ELS 2100 (neb=30°C , evap=50°C, gas=1.0 SLM) ELSD UV @ 220nm

  19. Advantages of Evaporative Light Scattering Detection • Universal: responds to all compounds in the mobile phase • Detects compounds that do not possess a UV chromophore (eg polymers, sugars) • Not dependent on spectroscopic properties of compound • Produces more uniform detection sensitivity for analytes

  20. Advantages of Evaporative Light Scattering Detection: Uniformity of Response Comparison of UV and ELS traces show that ELSD allows for a more uniform response than UV detection Column: PLRP-S 100Å 5µm, 150 x4.6mm Eluent A: 50% 0.1% TFA in Water : 50% 0.1% TFA in ACN Flow Rate: 1.0ml/min Inj Vol: 10µl Detector: PL-ELS 2100 (neb=30°C, evap=30°C, gas=1.4 SLM) UV-VIS @ 280nm

  21. Advantages of Evaporative Light Scattering Detection • Universal: responds to all compounds in the mobile phase • Detects compounds that do not possess a UV chromophore (eg polymers, sugars) • Not dependent on spectroscopic properties of analyte: • Produces more uniform detection sensitivity for analytes • Not susceptible to baseline drift during gradient elution, temperature or solvent pump fluctuations • ELSD compatible with a much wider range of solvents compared to RI and UV

  22. Fast Gradient, Fast Flow Rate Capability Sample: Indapamide (IND), Dibutyl phthalate (DBP) Column: PLRP-S 100Å 5µm, 50x4.6mm Eluent A: 0.05% TFA in Water Eluent B: 0.05% TFA in ACN Gradient: 5-95% B in 1 min Flow Rate: Increased from 2ml/min up to 5ml/min Detector: PL-ELS 2100 (neb=30°C, evap=30°C, gas=1.6 SLM) Note: IND is non-volatile, DBP is relatively volatile

  23. DBP IND 2ml/min 3ml/min 4ml/min 5ml/min min Fast Gradient, Fast Flow Rate Capability

  24. 2ml/min 3ml/min 4ml/min 5ml/min Fast Gradient, Fast Flow Rate Capability Stable baseline throughout the gradient PL-ELS 2100/2100 Ice can operate in 100% up to 5ml/min min

  25. Advantages of Evaporative Light Scattering Detection: Ideal Complement to LC-MS • Similar operating principles to LC-MS • Volatile buffers • Favors lower flow rates (ie 0.2-0.5 ml/min) • Can develop LC methods on PL-ELS 2100/2100 Ice then transfer to LC-MS • ELSD can provide supporting information when used in tandem with LC-MS

  26. Ideal Complement to LC-MS Sample Mixtureof known 1:1 ratio LC-MS results show ratio to be 3:1 UV-Vis result show ratio to be 10:1 PL-ELS 2100 results show ratio to be 1:1 (Response independent of optical properties)

  27. PL-ELS 2100/2100 Ice Sensitivity Limit of Detection LOD improved with lower eluent flow rates and smaller ID column Caffeine Loading 100ng 4.6 ID S/N = 4.4 Caffeine Loading 30ng 2.1 ID S/N = 11.5

  28. Routine operation of PL-ELS 2100 & PL-ELS 2100 Ice • FOR NON-VOLATILE SOLUTES • Evaporator temperature can be set to 80-120°C • PL-ELS 2100 • Gas flow kept to a minimum to maximise S/N • Compounds such as sugars, fats/oils, & surfactants. • FOR SEMI-VOLATILE SOLUTES • Evaporator temperature often set between 30-50°C • PL-ELS 2100 or PL-ELS 2100 Ice • Gas flow optimised according to mobile phase • Water @ 30°C requires 1.6SLM of gas • Pharmaceuticals (e.g. MW >300), antibiotics & nutraceuticals.

  29. Routine operation of PL-ELS 2100 Ice • FOR VOLATILE SOLUTES • Sub-ambient Evaporator temperatures required - 10-30°C • PL-ELS 2100 Ice • Gas flow optimised for sub-ambient temperatures and mobile phase • 100% Water @15°C requires 2.2SLM of gas • Compounds with high vapour pressures, low MW pharmaceuticals, pesticides, hydrocarbons

  30. Sub-Ambient Applications The S/N ratio for thermally sensitive compounds such as Acetanilide is improved at sub-ambient temperatures In addition, the response of compound’s with high boiling points and high volatility, such as Alkanes, is dramatically improved.

  31. Sub-Ambient Applications: Acetanilide (MW 135)

  32. Sub-Ambient Applications: Alkanes

  33. Improved accuracy of quantification at sub-ambient temperatures Quantity and purity analyses for pharmaceutical drugs typically use HPLC coupled with UV/MS/ELSD Only ELSD allows compound-independent calibration, provided gradient effects and physicochemical properties of analytes are accounted for. Volatility is the most important physicochemical property that limits the accuracy/sensitivity of ELSD. Hence, ELSD operating temperatures need to be as low as possible, to minimise volatility effects.

  34. Improved accuracy of quantification at sub-ambient temperatures Average Recovery 84% Average Recovery 28%

  35. Improved accuracy of quantification for semi-volatile compounds At 30°C, the average recovery across the four compounds was 28% At 16°C, the average recovery across the four compounds was 84% By operating at sub-ambient temperatures the loss of semi-volatile analytes is minimised, hence the accuracy of quantification is improved. The data also shows how small changes (2-4°C) in evaporator temperature can have dramatic effects on the response of semi-volatile compounds. For laboratories without a stable thermal environment, it is vital that the evaporator temperature is accurately controlled

  36. Ambient Applications: Pharmaceutical mixture Samples: 1. Acetanilide, 2. Indapamide, 3. Ibuprofen, 4. Dibutylphthalate Column: C18 5µm, 150x4.6mm Eluent A: 0.1% TFA in Water Eluent B: 0.1% TFA in ACN Gradient: 60-90%B in 5 mins Flow Rate: 1.0mL/min Detector: PL-ELS 2100 (neb and evap set at the same temperature, gas 1.8 SLM) Note: peak 2 is non-volatile, peaks 1, 3, 4 are relatively volatile

  37. Ambient Applications: Pharmaceutical mixture At high temperature, Peak 2 has better S/N but Peaks 1,3 & 4 are not detected At 30°C all four peaks are detected

  38. Ambient Application: Herbicides Sample: Mixture of 10 Phenylurea herbicides Column: C18 5µm, 250x4.6mm Eluent A: Water Eluent B: Acetonitrile Gradient: 10-80% B in 40 mins Flow Rate: 0.7ml/min Inj Vol: 20µl Detector: PL-ELS 2100 (neb=25°C, evap & gas flow varied)

  39. Environmental Application: Herbicides 50°C 70°C Sample integrity is preserved at lower operating temperatures 25°C

  40. Non-Volatile Application: Triglycerides in Natural Oils Sample: 2mg/ml Starflower Oil Column: C18 5µm, 250x4.6mm Eluent A: ACN Eluent B: DCM Gradient: 30-50% B in 40 mins; 50-90% in 2 mins, hold for 3mins Flow Rate: 1.0ml/min Inj Vol: 20µl Detector: PL-ELS 2100 (neb=40°C, evap=70°C, gas=1.4 SLM)

  41. PL-ELS 2100/2100 Ice:DMSO Transparency Sample: Pharmaceutical Mixture in DMSO Column: Thermo-Hypersil C8 5µm, 50x4.6mm Eluent A: Water Eluent B: Acetonitrile Gradient: 5-100% B in 5 mins Flow Rate: 1.0ml/min Inj Vol: 20µl Detector: PL-ELS 2100 Ice (neb=25°C, evap & gas flow varied)

  42. DMSO Transparency:Ideal for High Throughput Screening Loss of volatile species occurs as temperature is increased

  43. DMSO Transparency:Ideal for High Throughput Screening • The design of the PL-ELS 2100 Ice makes it transparent to • DMSO at 25-30°C • Fast eluting compounds are not masked by DMSO peak. PL-ELS 2100: neb=25°C, evap=30°C

  44. PL-ELS 2100/2100 Ice Control Software Control & Method Manager software supplied as standard Software control via a serial connection (RS232) on selectable COM port Method Manager utility allows the user to set up, edit and log defined methods which can then be downloaded to the PL-ELS 2100ICE The PL-ELS 2100/2100 Ice have 24bit digital outputs via the RS232 port to provide data acquisition via Galaxie™chromatography data system

  45. Benefits of Evaporative Light Scattering Detection Universal detector: independent of the optical properties of the solute Compatible with gradient elution Ideal for fast gradient elution - no solvent front removes the need for derivatization Compatible with chromatographic techniques such as MS and SFC Wide application area

  46. Benefits of the PL-ELS 2100 The PL-ELS 2100/2100 Ice provides all the typical advantages of ELSD, plus: • Compatible with eluent flow rates, up to 5ml/min • Detection limit in the low nanogram range • High sensitivity to semi-volatile compounds • DMSO transparency at ambient temperature • Extremely low dispersion for high resolution separations • Software control • Digital signal processing

  47. Additional Benefits of the PL-ELS 2100 Ice • Sub-ambient operation down to 10°C for maximum sensitivity to volatile compounds • Active heating/cooling provides rapid equilibration between analyses. • Improved accuracy of quantification.

  48. PL-ELS 2100 Ice ‘Lock out’ Specs • Sub-ambient operation down to 10°C • High sensitivity to semi-volatile compounds • DMSO transparency at ambient temperature • Extremely low dispersion for high resolution separations • Compatible with eluent flow rates, up to 5.0ml/min • Rapid thermal equilibration • Easy to use • Extremely small footprint, stackable

  49. PL-ELS 2100 Specifications Light source: LED 480nm Detector: Photomultiplier tube Nebuliser temperature: ambient to 90°C in 1°C increments Evaporator temperature: ambient to 120°C in 1°C increments Gas flow rate: up to 3.25 SLM Gas pressure: typical 60-100psi, maximum 100psi Eluent flow rate: up to 5 ml/min Output: Analogue: 0-1V FSD Digital: 24bit, 10Hz using serial connection Communications: serial I/O (RS232), contact closure, TTL Power requirements: 90/120V AC or 220/250V AC 50/60 Hz Dimensions: 200x450x415mm (wxdxh) Weight: 11kg Part No. PL0860-0110 (110v), PL0860-0240 (240v) 200mm 200mm 415mm 450mm 450mm

  50. PL-ELS 2100 Ice Specifications Light source: LED 480nm Detector: Photomultiplier tube Nebuliser temperature: ambient to 90°C in 1°C increments Evaporator temperature: 10 to 80°C in 1°C increments Gas flow rate: up to 3.25 SLM Gas pressure: typical 60-100psi, maximum 100psi Eluent flow rate: up to 5 ml/min Output: Analogue: 0-1V FSD Digital: 24bit, 10Hz using serial connection Communications: serial I/O (RS232), contact closure, TTL Power requirements: 90/120V AC or 220/250V AC 50/60 Hz Dimensions: 200x450x415mm (wxdxh) Weight: 13kg Part No. PL0860-1110 (110v), PL0860-1240 (240v) 200mm 200mm 415mm 450mm 450mm

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