Fast, Simple QA/QC of Milk Powder Formulations using FTIR Spectroscopy. Rob Wills Product Specialist Molecular Spectroscopy

Transcription

1 Fast, Simple QA/QC of Milk Powder Formulations using FTIR Spectroscopy Rob Wills Product Specialist Molecular Spectroscopy

2 Agilent Molecular Spectroscopy Portfolio

3 Agilent Molecular Spectroscopy Portfolio 2011

4 Agilent Cary introduced September 2011 An entry-level FTIR that will change the way analysts approach routine infra-red measurements! Designed for a wide range of markets, in particular, Chemicals QA/QC, Pharma QA/QC and Academic Teaching

5 MicroLab Method driven, guided sampling so simple and intuitive that anyone can use it

6 Near-IR μm, cm -1 Overtones and combinations Commonly used in food industry Commodity measurements Protein, water, fat, carbohydrate Food production, esp. meat, grains and milk Mid-IR (FTIR) μm, cm -1 Fundamental vibrations Mid-IR gaining use in food industry More sensitive and specific (higher information content) Lends itself to many different applications

7 - FT-IR analysis is SIMPLE to perform - FT-IR can require very little to NO SAMPLE preparation - Results are available within SECONDS to MINUTES - Powerful tool for analysis of any GAS, LIQUID or SOLID - The method is VERSATILE (can accommodate various sample sizes and types) - Provides both QUANTITATIVE and QUALITATIVE results - FT-IR provides incredibly ACCURATE results - FT-IR analysis CAN BE NON-DESTRUCTIVE - FT-IR spectroscopy is an AFFORDABLE method

8 QA/QC of Dairy Powders using the Agilent Cary 630 ATR-FTIR Analyser Authors: Zubair Farooq and Ashraf A. Ismail McGill University, Quebec, Canada Publication number: EN Publication date: November 2012

9 Milk protein powder samples including α-lactalbumin, β-lactoglobulin, glycomacropeptide, milk protein concentrate, WPI, WPC, caseins and caseinates were obtained from different suppliers. A spectrum of each sample was obtained using the Cary 630 FTIR equipped with diamond ATR interface. Spectra were collected using 64 scans at 4cm -1 resolution approx. 30 secs measurement time.

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11 The differences among the spectra are hard to distinguish by the naked eye. All four protein types can be immediately characterized and differentiated with the built-in spectral analysis capability of the MicroLab FTIR software. Correct identification of an unknown dairy powder as α-lactalbumin by the MicroLab FTIR software

12 Determination of Sucrose Levels in Infant Cereals using the Cary 630 FTIR-ATR Authors: Chih-An Lin, Huseyin Ayvaz, and Luis E. Rodriguez-Saona Ohio State University, Columbus, USA Publication number: EN Publication date: July 2015

13 Sucrose is a key additive in many breakfast cereals. It is used to improve taste and appearance, especially when added in the form of a coating, but due to health concerns there is a need to measure and control the amount of sugar present. Chromatography or wet chemistry are often used for this purpose, however, these methods are time-consuming and require additional sample preparation, hence there is substantial interest in methods for measuring sugar that eliminates some of the issues associated with traditional analytical methods. FTIR can be used as a simple alternative, with the following benefits... The speed of analysis is greatly increased. No sample dilution or preparation other than grinding is required. The level of user experience required to obtain reliable answers is reduced. Samples do not have to be sent to a remote lab for analysis, i.e. analysis can be performed where and when the measurement needs to be made.

14 Chemometrics software is needed to overcome problems of spectral overlaps inherent in a complex sample matrix such as this.

15 Independent external validation set of 20 additional samples shows high correlation for sucrose (> 0.95) when compared with data obtained by the HPLC reference method. 64 co-averaged scans collected at 4cm-1 resolution (30 secs). Spectra were normalized, and second-derivative transformed through a Savitsky-Golay second order polynomial filter with a 35- point window, prior to the partial least squares (PLS) regression analysis.

16 Detection of Adulteration in Milk Products using FTIR Author: Luis E. Rodriguez-Saona Ohio State University, Columbus, USA Publication number: EN Publication date: February 2013

17 Application note relates to adulterants in bovine milk, measured in both liquid and powder (freeze dried) form. Again, chemometric software analysis is used to identify and classify the type of adulterant at levels as low as 3% v/v. Liquids measured in transmission Solids measured using ATR

18 Companies using the milk for further production (e.g. of powdered infant formula) normally check the protein level through a test measuring nitrogen content. The addition of melamine increases the nitrogen content of the milk and therefore its apparent protein content. A study in 2011* showed how FTIR spectra collected in the mid infrared (MIR) region between 4000 and 600 cm 1 could be used to detect melamine contamination. FTIR data was processed using regression and multivariate analysis and spectral changes in the amide I and II regions ( cm 1 ) and the fingerprint region ( cm 1 ) were used to identify and quantify contamination and provide a model for future analysis. * Balabin RM1, Smirnov SV., Melamine detection by mid- and near-infrared (MIR/NIR) spectroscopy: a quick and sensitive method for dairy products analysis including liquid milk, infant formula, and milk powder., Talanta Jul 15; 85(1):562-8.

19 A more recent study by S. Jawaid et al published in Food Chemistry 141 (2013) demonstrated the use of FTIR-ATR for rapid and accurate detection of melamine adulteration with excellent detection limits reaching the safety limits set by EU and US FDA.

20 Agilent 5500 Dedicated Analyser for routine use by non-skilled personnel outside of the lab, for example.. Factory floor Gatehouse Agilent 4500 Truly portable, battery operated system for routine use by non-skilled personnel outside of the lab, for example... Anywhere!

21 Stable Isotope Technique for Assessment of Breast Milk Intake Using Agilent 4500 Field Portable FTIR Authors: Alan Rein / Frank Higgins Agilent USA * Prof. Thomas Preston SUERC, Glasgow, UK * IAEA Seibersdorf, Austria Publication number: EN Publication date: December 2013

22 Historically, the method to assess intake of breast milk was to simply weigh the baby before and after feeding. Not only was this inaccurate, but it was also very time consuming and can adversely affect feeding patterns. O-D absorbance band measured using 100µm pathlength Plot of D 2 O concentration measured by IRMS and Agilent 4500 series FTIR shows excellent correlation In short, a dose ( bolus ) of D 2 O is given to the mother and her Deuterium levels read via FTIR at day 1, 2, 3, 4, 13,14. The baby, who ingests the Deuterium enriched water from the mother through breastfeeding, is also monitored from his/her saliva.

23 Sample measurement is quick and simple using the patented TumblIR interface. The measured D 2 O in units of mg/kg are entered into an IAEA spreadsheet, and since the rate of decay of D 2 O is accurately known, we can very accurately calculate the amount of breastmilk consumed.

24 Summary FTIR can be used for a wide range of applications from simple screening of incoming raw materials to delivery of fast, accurate quantitative results. Measurements are fast, simple to make, highly reproducible and can be made outside of the lab just as easily as inside the lab.