FT-NIR Spectroscopy for Food and Natural Heath Products Analysis. Subtitle
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1 FT-NIR Spectroscopy for Food and Natural Heath Products Analysis Subtitle
2 If you re going to need a year to train a horse to locate contriband pick a musical one We all know that exceptionally welldesigned, manufactured, delivered and installed instruments do not (necessarily) make great Analytical Methods
3 If you re going to need a year to train a horse to locate contriband pick a musical one We all know that exceptionally welldesigned, manufactured, delivered and installed instruments do not (necessarily) make great Analytical Methods Clever people make great Analytical Methods A clever person can make sound and successful methods with the simplest of tools, or largely incomplete tools for the job, by learning to apply them to the greatest advantage
4 If you re going to need a year to train a dog to locate contriband pick a musical one However, given the chance, clever people will pick exceptionally well designed, manufactured, delivered and installed instruments because it will make their job a whole lot easier! Clever people together with great instruments can make exceptional Analytical Methods
5 If you re going to need a year to train a dog to locate contriband pick one with a great great nose
6 If you re going to need a year to train a dog to locate contriband pick one with a great great nose - and an inclination to use it!
7 The MPA Multi-Purpose Analyzer multiple measurement accessories for different sampling techniques: Fiber Optic Probes Integrating Sphere Transmission Unit automated Sample Wheel Sample Rotator software controlled measurement accessories selection full line of sampling accessories and options
8 Unique Features of Bruker MPA Custom-made Instrument: Each customer buys exactly the instrument that matches his application. There is no need to purchase anything that is not wanted or needed. MPA basic configuration MPA fully equipped
9 Maximum Flexibility: Sample Compartment Fiber Optic Probes External Integrating Transmission i Sphere
10 The MATRIX-F compact Process Spectrometer with Rocksolid TM Interferometer modular Design robust, rugged and waterproof highest Reliability high long-run Stability high measuring Accuracy unrestricted Method Transfer possible all Components in 19 Geometry
11 The MATRIX-I based on the optical module of MATRIX-F robust, rugged and waterproof fixed, gold-coated Integration Sphere vibration and temperature insensitive at-line and in-line Installation used for heterogeneous and coarse- grained materials much better light efficiency than probes
12 Calibration Transfer: The exceptional performance of the instrument t ensures a smooth calibration transfer not only to other MPA instruments but also to the MATRIX process spectrometers.
13 Calibration Transfer: The exceptional performance of the instrument t ensures a smooth calibration transfer not only to other MPA instruments but also to the MATRIX process spectrometers. One Calibration one million measurements!!!
14 Spectrometer Calibration at H 2 0 Vapor Bands. 025 Single beam spectr ra resolution = 25 cm -1 resolution = 2 cm target: 7.306,74 cm Wavenumber / cm -1
15 OPUS spectroscopy software: Flexible software, optimized i for the special demands of the FT- NIR technology. Various software packages enable a qualitative as well as a quantitative analysis of the samples. Modular design, additional software packages can seamlessly be integrated in the existing OPUS suite. The customer is able to use all software functions without any restriction.
16 OPUS/IDENT: Identification software with factor analysis as well as with the Euclidian distance calculations Hierarchical libraries offer the identification of samples in multiple levels: large libraries possible (>2,000 samples) hi h d f ti high degree of separation, even with very similar products!
17 OPUS/QUANT: Quantification software with automated calibration function: user defined optimization regions three different optimization functions even inexperienced users to generate calibrations at a push of a button the process of time consuming method generation and optimization is reduced to a minimum
18 OPUS/LAB: Easy-to-use interface for the laboratory: even inexperienced users can use OPUS/LAB pre-defined order of events no mistakes freely configurable to the needs of your users
19 Full GMP and 21 CFR part 11 compliance: OPUS in combination with the MPA complies with regulations issued by ISO, ASTM, FDA and USP. full GMP capabilities like multiple security levels, non-editable data files and complete audit trails. electronic records and signatures ensure 21CFR11 compliance. Bruker Optics is a certified supplier and was audited by several pharmaceutical companies.
20 Training: free training after the installation of the instrument German training i courses twice a year English training course once a year personal in-house training at the customer s facility on demand every instrument is supported by an expert who is available for you when required
21 Areas of Application Food & Feed Chemistry Petro & Polymer Pharma Cosmetics
22 Sample Forms Liquids Emulsions Pastes Resins Seeds Powders Tablets Paper Granulates Phials Foils Coatings
23 Limits of NIR Technology Detection of C-H-, N-H-, O-H- and C=O-vibrations (mainly examination of organic compounds). The NIR-technique is currently not suitable for trace analysis Usually in the percentage range, sometimes down to 0.1% Examination of complex mixtures (> 5-7 components) usually demands a higher calibration effort. NIR is often not suitable for the identification of unknown samples.
24 How does a quantitative analysis work? - Setting up a Calibration Units Absorbance Wavenumber cm-1 Measurement of spectra with known concentration Spectra - Quantifying unknown Samples Factors 1 2 Calculation of the spectral parameters Analysis r r r r r r r r r rr rr r r r Reference Building up a calibration curve 1.5 % Comp. A 34 % Comp. B 62% Comp. C Measurement of unknown samples Analysis of Determination ti of unknown spectrum concentration(s)
25 Pharmaceutical Applications Subtitle
26 NIR Applications of Pharmaceuticals Substance Identification in the Receipt of Goods Quantification of active Materials (API s) auxiliary Materials Fillers in Powders, Capsules, Tablets or Vials Water Content in Powders Drying Processes Blending Solvent Recovery...
27 Calibration of active Ingredients Calibration of Ibuprofene Paracetamol in Tablets measued with External Transmission Unit
28 Ibuprofen in Tablets NIR valu ue / % reference value / %
29 Paracetamol in Tablets NIR valu ue / % reference value / %
30 Calibration of active Ingredients Results: R 2 Range RMSECV Ibuprofene % ± 0.3% Paracetamol % ± 0.3%
31 Ingredients of Vitamin Solutions Calibration of Methanol Water Sugar in Vitamin B2 Solution measured with 1 mm Transmission Probe
32 Methanol in Vitamin B2 Solution NIR valu ue / % reference value / %
33 Water in Vitamin B2 Solution 50 NIR valu ue / % reference value / %
34 Sugar in Vitamin B2 Solution 10 9 NIR valu ue / % reference value / %
35 Calibration of Ingredients Results: R 2 Range RMSEP Methanol % ± 0.18% Water % ± 0.15% Sugar % ± 0.11%
36 Cosmetics Applications Subtitle
37 Calibration of Shampoo Calibration of Wash Active Substances in Shampoo measured at 30 o C in the Sample Compartment
38 Wash Active Substances in Shampoo 285 NIR value / mmol/ /kg reference value / mmol/kg
39 Calibration of Shampoo Results: R 2 Range RMSECV WAS ± 2.5 [mmol/kg]
40 Surfactant in aqueous Solution 80 NIR va alue / % reference value / %
41 Food & Feed Applications Subtitle
42 MPA with Integrating Sphere and Sample Compartment
43 MPA Int.Sphere/Sample Comp./Transmission Unit
44 MPA with Petri Dish Rotator
45 MPA with Rotator and Transmission Unit
46 Starter Calibrations for Food Aapplications
47 Food Starter Calibrations for turn-key solutions Multiple Packages B-DAI-M Dairy B-MEA-M Meat B-OIL-M Edible Oils Price List Single Package B-DAI-S B-MEA-S B-OIL-S Dairy Meat Edible Oils
48 NIR Starter Calibration Packages: Dairy Liquid Milk and Milk Products in Transmission (1mm flow cell) Raw and whole milk Whey Whey concentrate Whey protein concentrate Whey cream and cream Lactose Concentrate Brine (Mozzarella) Cleaning and disinfection solvents
49 Starter Calibration for Milk Powder Calibration of Fat Protein Moisture Ash Lactose in Milk Powder Measured on the sphere with IN311/C + IN311-S
50 Measurements of melamine in milk powder Absorbance Units Pure milk powder (red) Pure melamine (blue) Wavenumber cm
51 Measurements of melamine in milk powder Admixture of melamine powder to standard milk powder from % Absorbance Units Peak at 6812cm Wavenumber cm
52 Measurements of melamine in milk powder ion / % NIR R-Predict NIR-Calibration melamine in milk powder R² = RMSECV= True Value / % 52
53 Measurements of melamine in liquid milk Absorbance Units Liquid milk of 1.5% and 3.5% of fat with admixture of melamine from 0.05% - 0.3% Wavenumber cm
54 Measurements of melamine in liquid milk 0.31 NIR-Calibration melamine in liquid milk ion / % NIR R-Predict R² = RMSECV= True Value / % 54
55 Measurement: Oils in Sample Compartment Instrumentation: - MPA Multi Purpose Analyzer - MPA-C: Sample Compartment - IN601/CU: heatable Vial Holder - IN601C08: Insert for Vials - IN430: disposable 8mm Vials Resolution: 8 cm -1 No. of Scans: 32 Scans Temperature: 50 o C
56 External Heating Block
57 Universal Calibrations Property Data Set Performance Name Unit n Min Max Rank R 2 SEP Iodine Value IV Trans Fatty Acids % TFA low range % These calibrations should normally work without further adaptation with common customer samples.
58 Measurement: IV value of Oils Prediction vs True / IV / Independent Validation The result of cross-validation shows that the NIR spectra of fats and oils have a high correlation with their IV (R 2 =99.99%), and the accuracy of NIR analysis expressed in root mean square error of cross-validation is about 1 and in root mean square error of prediction is 1 for independent validation samples.
59 Measurement: Trans content in Fats/Oils trans content was expressed as %FA Universal trans content calibration covers trans content from 0 to 56%FA
60 Starter Calibrations Property Data Set Performance Name Unit n Min Max Rank R 2 SEP Anisidine Value AnV Free Fatty Acids % C16:0 (Palmitic Acid) % C18:0 (Stearic Acid) % C18:0 (Stearic Acid) % C18:1 (Oleic Acid) % C18:2 (Linoleic Acid) % C18:3 (Linolenic Acid) % Customer samples should be added for optimum performance.
61 Global calibrations for the Food and Feed Industry
62 Mix of ingredients for animal feed Energy Source wheat, barley, corn, oats, fat, molasses etc. Vegetable Protein soya, rapeseeds, sunflower seeds etc. Crude Fibers wheat bran, sugar beet pulp, trester etc. Minerals lime, phosphate, salt, trace elements etc. Vitamins
63 Task of a Nutritionist: the best feed in constant quality for the lowest price For the optimization of the mixed feed the Nutritionist needs to know the property values of the raw materials for: protein, moisture (dry matter), fiber, oil (fat) and ash. For this task classical wet chemistry is slow and expensive! This is a NIR task!
64
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