Collagen and bone fat are important resources in the food industry. It is essential that these primary products are odor- and taste free. Extensive de-odourization processes are used during bone fat & collagen processing to eliminate any off-flavors that might be present. Regular sensory evaluation performed by specially trained panels in combination with GC-MS analysis ensures product quality is not compromised.

1. ANALYSIS OF MALODOR DURING
Renton (Ewan McGregor) // Trainspotting
BONE FAT PROCESSING

2. 2
Knowledge is our biggest asset.
Combining it, leads to new insights, solutions and approaches.
The goal of this newsletter is to provide
the creative sparks to ignite serendipitous thoughts, ideas and insights.
Look at www.is-x.com for more valuable resources or give us a call.
Joeri Vercammen, Ph.D.
j.vercammen@is-x.com

3. TABLE OF CONTENTS
Cover article
News
Pages 4-6
01 02
Reflections
Xtandards
Pages 7-11
03
Network News
ure X
Pages 12-14
04
News Flash
a
Pages 15-24
05
Gadgets &
Innovations
Pages 25-27

4. PART 1
Cover article

5. 5
MALODOR ANALYSIS
Collagen and bone fat are important
resources in the food industry. It is
essential that these primary products are
odor- and taste free. Extensive de-
odorization processes are used during
bone fat & collagen processing to eliminate
any off-flavors that might be present.
Regular sensory evaluation performed by
specially trained panels in combination
with GC-MS analysis ensures product
quality is not compromised.
SPME enriches trace levels components and
makes them more amenable to GC.
“
Recent analysis of de-odorized bone fat at NIZO indicated that low
boiling point aldehydes, such as pentanal, hexanal and heptanal, are
present that were not detected by the GC-MS method currently in use.
In this study, it is evaluated to which extent SPME in combination with
the newest generation GC/MS is able to provide sufficient sensitivity to
identify potential malodors in the headspace of de-odorized bone fat and
hydrolyzed collagen.

6. RT: 0.00 - 36.09
0 2 4 6 8 10 12 14 16 18 20 22 24 26 28 30 32 34 36
Time (min)
0
5
10
15
20
25
30
35
40
45
50
55
60
65
70
75
80
85
90
95
100
RelativeAbundance
30.22
30.32
21.27
30.66
27.60
31.66
23.87 30.04
27.18
21.91
29.66
35.9334.35
18.47
3.082.80 26.17
20.64
3.74 4.95 17.675.60 12.31 13.08 24.4314.92 23.376.73 10.36
NL:
3.00E8
TIC MS
collageen_i
n_nacl
MALODOR ANALYSIS
The chromatogram displays the result of the analysis of a hydrolysed collagen sample after 30 min static enrichment with a
PDMS/Carboxen fiber at 55°C. Significant levels of sulfur components such as carbon disulfide and dimethylsulfide as
well as several aldehydes could be identified.
In a second phase of the project it will be
evaluated whether alternative injection
techniques are capable of reaching similar
detection limits.

7. PART 2
Reflections

8. 8
OLIVE QUALITY
The last couple of months, quite some
rumor has been associated with the quality
and authenticity of olives and olive oil,
respectively.
• We have participated in a European call
under the Horizon 2020 framework that
was aimed at determining the
authenticity of olive oils
• We are currently in discussion with a
Spanish university to evaluate the
feasibility of SIFT-MS for this purpose.
• For those of you that forgot, in Refocus
03//2014, I refer to an application that
applies direct analysis of edible oils using
direct TD.
In this application, we did not focus on oil quality but rather
on the analysis of olives after fermentation, so-called Spanish-
style olives.
These olives are prepared by soaking in lye (dilute NaOH, 2-4%) for 8–
10 hours. After rinsing with water, they are transferred to fermenting
vessels full of brine at typical concentrations of 8-12% NaCl. Here, their
typical flavor develops by bioconversion of sugars into acids and other
aromatic compounds through action by natural microbiota that occur
on the olives.
Many organisms are involved, usually reflecting
the local conditions or "Terroir" of the olives.
“

9. Off-flavors may appear because of uncontrolled conditions like low acidity or salinity.
By analyzing olive aromagrams, three off-flavors have been identified and for each of them target indicative compounds.
The first default is characterized by a strong persistent odor and taste, high concentrations of propionic acid and the
simultaneous occurrence of cyclohexane carboxylic acid. The second is correlated with high levels of 3-hydroxy-butan-2-
one and a buttery aroma and finally the last one which is characterized by a rancid odor and the occurrence of n-butanoic
acid. For each compound, threshold values have been determined. Table 1 shows the maximum allowable level for each
compound.
We have developed a GC method that applies headspace injection after salination and acidification to measure the
components presented in Table 1 alongside several other marker components.
9
Compound Concerned off-flavour Threshold value, mg/L
Propionic acid Propionic fermentation 300
Cyclohexane carboxylic acid Propionic fermentation 2
Butyric acid Butyric fermentation 50
Acetoin Butanediol fermentation 500
OLIVE QUALITY

10. 10
The analysis of airborne aldehydes and
ketones first involves collection of the analytes
by passing air through a cartridge containing
2,4-dinitrophenylhydrazine (DNPH). As the
air passes through the cartridge, the
analytes react with the DNPH to form
hydrazones which are immobilized on
the cartridge. The cartridges are then eluted
with solvent and the DNPH derivatives
determined using HPLC with UV detection.
10
AUTOMATED ANALYSIS OF DNPH-ALDEHYDES
A RSH-type robotic sample handler was equipped with a
special tray to hold DNPH cartridges, enabling efficient
automation of the entire process of desorbing the analytes
and injecting the eluate into the LCUV system.
Automating the desorption of these cartridges significantly
improves both accuracy and reproducibility. In addition, the
risk of operator error is reduced. Prep ahead software
functioning enables desorption of a cartridge during the
chromatographic separation of the previously injected
sample. This means that the next sample is always prepared
and ready to be injected as soon as the HPLC system has
completed the previous analysis, ensuring maximum sample
throughput.

11. 11
Just recently, Ionicon presented their most
recent add-on for their high end PTR-TOFMS
instrument. Although principally positioned as
a direct MS technique, PTR-TOFMS seems to
suffer from matrix interference more than
anticipated. What’s going on?
PTR-TOFMS is a very sensitive device that
permits low PPT detection of volatile
components in air. It applies ionization with
H3O+ ions, which are generated in situ.
Although PTR-ionization is substantially
softer than electron impact, it still
suffers from analyte fragmentation
giving rise to abundant spectra,
particularly in complex samples.
11
THE RISE AND FALL OF PTR-TOFMS
Initially, this intricate spectral complexity was dealt with by
applying TOFMS in high resolution mode. Now, Ionicon has
announced a new feature in which PTR-TOFMS analyses is
preceded by a fast GC analysis, by means of an additional
module which is put just in front of the instrument.
In that way the PTR-TOFMS has evolved from an
elegant analytical solution (with dedicated
applications) to an over-engineered device without
any added value. When selectivity is an issue and you are
interested in analyzing VOC on-line at sub-PPB levels:
consider SIFT-MS in stead of PTR-MS. Ionization is much
softer compared to PTR while triple ion selectivity guarantees
selective detection, irrespective of sample complexity. And
when you still need a GC/TOFMS then have a look at the
BenchTOF instrument from Markes.

12. PART 3
Network news

13. 13
Stable TiO2–USY zeolite composite coatings for efficient adsorptive and photocatalytic
elimination of geosmin from water
Summer 2013.
Nikki Janssen joins our team for a couple of weeks. Nikki is a Ph.D. student from Leuven University and she developing
new materials to remove geosmin from water. Geosmin is a tainting component that develops in water due to bacterial
proliferation. Together we have developed a GC/MSMS method that permits quantitative analysis of geosmin at low PPT
levels in water by means of SPME.
Winter 2015
The results of this work have recently been accepted for publication in the Journal of Materials Chemistry.
http://pubs.rsc.org/en/content/articlelanding/2014/ta/c4ta05941g#!divAbstract
GEOSMIN ANALYSIS AT PPT LEVELS
“

14. 14
New lab for asphalt research
UAntwerp and bitumen manufacturer NYNAS redesigned the infrastructure of the research group ‘Road
Construction’ (wegenbouwkunde). The refurbished laboratories, which are located at the Campus Paardenmarkt, allow for
top notch scientific research particularly aimed at:
• Lowering the production temperature of asphalt
• Recycling of old roofing in asphalt and
• Noise-reducing top layers.
IN THE PRESS
“

15. PART 4
News flash

16. 1616
Volatile aldehydes identified as markers for breast cancer
Breath is beginning to take on increasing importance in the clinical world as its
potential for diagnosing various diseases is unfolding, especially cancers. There
have been a number of studies describing how particular volatile compounds that
are exhaled by patients can predict the presence of lung cancer. However, cancers
in other parts of the body that are disconnected from the lungs can also produce
signal metabolites that end up in the breath, such as colorectal, prostate, and head
and neck cancers.
Breath from patients with breast cancer and benign breast tumors was compared
with that from healthy people. They blew through a cardboard mouthpiece into a
sample device comprising an inert plastic syringe with a one-way valve piston
which trapped the last portion of the breath without contamination from breath
from the mouth or bronchial tubes. The trapped breath was transferred to a Tedlar
bag for storage before being sampled with a glass syringe and injected onto the
GC/MS system. The aldehydes were confirmed from their retention times and
mass spectra and measured by integrating three ions each from the extracted ion
chromatograms.
BREATH FOR BREAST CANCER
http://www.separationsnow.com/details/ezine/1495316b15b/Breath-for-breast-cancer-Volatile-aldehydes-for-diagnosis.html?&tzcheck=1
“

17. Headspace quantification of pure and aqueous solutions of binary mixtures of key volatile
organic compounds in Swiss cheeses using SIFT-MS
SIFT-MS was used for the headspace analysis of VOCs commonly found in Swiss-type cheeses. Headspace (H/S)
sampling and quantification checks using SIFT-MS and further linear regression analyses were carried out on twelve
selected aqueous solutions of VOCs. Five binary mixtures of standard solutions of VOCs were also prepared and the H/S
profile of each mixture was analyzed.
A very good fit of linearity for the twelve VOCs (95% confidence level) confirms direct proportionality between the H/S and
the aqueous concentration of the standard solutions. Henry’s Law coefficients were calculated with a high degree of
confidence. SIFT-MS analysis of five binary mixtures showed that the more polar compounds reduced the H/S
concentration of the less polar compounds, while the addition of a less polar compound increased the H/S
concentration of the more polar compound.
17
Rapid Commun. Mass Spectrom. 2015, 29, 1–10
CHEESE ANALYSIS
“

18. Xenon has been considered a prohibited substance according to WADA regulations in
September 2014. Its analysis from common specimens of routine sports drug testing is
desirable
18
Rapid Commun. Mass Spectrom. 2015, 29, 1–6
THE ROLE OF XENON IN DOPING
Urine was enriched to saturation with xenon,
sequentially diluted, and the target analyte was
detected as supported by the internal standard d6-
cyclohexanone by means of GC/MSMS using
headspace injection.
Three major xenon isotopes at m/z 128.9, 130.9 and
131.9 were targeted in (pseudo) selected reaction
monitoring mode enabling the unambiguous
identification of the prohibited substance.
Xenon was traceable in enriched human urine
samples down to the detection limit of approximately
0.5 nmol/mL. The intraday and interday imprecision
values of the method were found below 25%, and
specificity was demonstrated by analyzing 20 different
blank urine samples that corroborated the fitness-for-
purpose of the analytical approach to unequivocally
detect xenon at non-physiological concentrations in
human urine. The patients’ urine specimens returned
’xenon-positive’ test results up to 40 h post-
anesthesia, indicating the limits of the expected
doping control detection window.
“

19. 19
NEW ASTM STANDARD
The presence of ethylene glycol in in-service motor oil indicates that antifreeze coolant has leaked into the crankcase of an
internal combustion engine. Such leakage leads to engine wear problems. A new ASTM International standard will be used
to effectively determine whether glycols are present in motor oil. The new standard is D7922, Test Method for
Determination of Glycol for In-Service Engine Oils by Gas Chromatography. The standard will be used for
ethylene glycol detection by many types of companies that use large industrial engines, including:
• Trucks
• Earth moving machinery
• Railway trains
• Ocean-going ships
• Military vehicles
• High performance race cars
The test method describes an analysis for ethylene glycol
that looks for a single component buried in the complex
matrix of engine oil. A dirty used oil sample is directly
reacted with a chemical that will derivatize the ethylene
glycol to form another compound, ethylene glycol
phenylboronate, or EG-PBA. For more information, please
visit: http://www.astm.org/Standards/D7922.htm

20. If food flavor is not as expected, it can damage consumer confidence and give the perception of poor quality. Setting
analytical standards of what constitutes an acceptable flavor can be challenging, and while methods based on total volatiles
or specific marker compounds can be a useful quality control check, a more investigative approach is often required.
Determination of taints and off-flavors can be particularly challenging as the compounds are often
unknown and may be present at extremely low levels (sub ppb).
FOOD TAINTS & FLAVORS
In a recent article that appeared in LCGC, Kathy Ridgway discusses the
analytical methods available for taint and flavor analysis and highlights the
approaches taken to identify compounds responsible for the off-flavors.
The following topics are discussed:
• Instrumental Analysis
• Gas Chromatography–Olfactometry (GC–O)
• E-nose Technologies
• Flavor Release — Real-time Volatile Analysis
• Consumer Perception and Sensory Evaluation
• Sample Preparation and Extraction
• Liquid-based Extraction
• Headspace Extraction
• Solid-Phase Microextraction (SPME)
• Stir-Bar Sorptive Extraction (SBSE)
“
http://www.chromatographyonline.com/food-taints-and-flavours-investigative-approach

21. 21
PISTON-CYLINDER LLE
Determination of furfurals in Manuka honey using piston-cylinder LLE and GC
A rapid analytical approach for the direct measurement of furfurals such as
2-furfural and 5-methyl-2-furfural at parts-per-billion level in Manuka
honey is described. The approach employs a piston-cylinder based
liquid–liquid extraction device using chloroform extraction
solvent.
This device substantially reduces extraction time by a factor of 120 times
compared to solid phase micro-extraction and reduces solvent consumption by
a factor of 25 times compared to liquid–liquid extraction with mechanical
agita-tion. A recently commercialised capillary column offering a high degree
of inertness permits separation and detection of the analytes at ultra-trace
level without derivatisation. Repeatability of retention times for all compounds
is less than 0.1% (n = 20). The compounds cited can be analysed over a range
from 1 ng/g to 10 g/g in honey with a 5 ng/g limit of quantification (LOQ) and
correlation coefficients of at least 0.999.
http://www.sciencedirect.com/science/article/pii/S0021967314013041
“

22. 22
SMART(PHONE) DATAPROCESSING
Barcode-Like Paper Sensor for Smartphone Diagnostics
This study introduced a barcode-like design into a paper-based blood
typing device by integrating with smartphone-based technology. The
concept of presenting a paper-based blood typing assay in a barcode-like
pattern significantly enhanced the adaptability of the assay to the
smartphone technology. The fabrication of this device involved the use of
a printing technique to define hydrophilic bar channels which were,
respectively, treated with Anti-A, -B, and -D antibodies.
These channels were then used to perform blood typing assays by introducing a blood sample. Blood type can be visually
identified from eluting lengths in bar channels. A smartphone-based analytical application was designed to read the bar
channels, analogous to scanning a barcode, interpret this information, and then report results to users. The proposed
paper-based blood typing device is rapidly read by smartphones and easy for the user to operate. We envisage that the
adaptation of paper-based devices to the widely accepted smartphone technology will increase the capability of paper-
based diagnostics with rapid assay result interpretation, data storage, and transmission.
http://pubs.acs.org/doi/abs/10.1021/ac503300y
“

23. 23
AUTOMATED LLE
Gas Pressure Assisted Micro-LLE Coupled Online to Direct Infusion Mass Spectrometry
In the field of bioanalysis, there is an increasing demand for miniaturized, automated, robust sample pretreatment
procedures that can be easily connected to direct-infusion mass spectrometry (DI-MS) in order to allow the high-
throughput screening of drugs and/or their metabolites in complex body fluids like plasma. LLE is a common sample
pretreatment technique often used for complex aqueous samples in bioanalysis. Despite significant developments that
have been made in automated and miniaturized LLE procedures, fully automated LLE techniques allowing high-
throughput bioanalytical studies on small-volume samples using direct infusion mass spectrometry, have not
been matured yet. Here, the authors from Leiden University introduce a new fully automated micro-LLE technique based
on gas-pressure assisted mixing followed by passive phase separation, coupled online to nanoelectrospray-DI-MS.
http://pubs.acs.org/doi/abs/10.1021/ac502582f
“

24. 24
TO-17: A Single-Method Approach for the Analysis of VOC and sVOC in Air Using TD-
GC/MS
TD 2.0: VOC AND SVOC IN A SINGLE RUN
This article describes a new, single method to replace the
two-method approach using United States
Environmental Protection Agency (EPA) Methods TO-15
and TO-13A for the analysis of both volatile organic
compounds (VOC) and semivolatile organic compounds
(SVOC) in air.
The study presents evidence that these components can be
determined using one analytical method that follows EPA
TO-17 capturing the volatile compounds in addition to
recovering the heaviest components, such as
benzo[ghi]perylene. The investigation also takes a look at
some of the 50 additional compounds that are expected to
be added to this list in the near future.
The advantages of replacing Methods TO-13A and
TO-15 with Method TO-17 for the analysis are the
cost savings to both the laboratory and the client,
and that TO-17 requires no sample preparation once the
samples arrives at the lab. The tubes are simply placed on
the autosampler and analyzed. After starting the thermal
desorber, the instrument automates the process of
desorbing the analytes from the tube, and injecting the
sample into the analytical column for detection and
analysis by GC–MS. In addition, the data generated from
the site evaluation , will show that thermal desorption is
more efficient than Soxhlet extraction and also requires
significantly less operator intervention.
http://www.chromatographyonline.com/single-method-approach-analysis-volatile-and-semivolatile-organic-compounds-air-using-thermal-desorp?rel=canonical
“

25. PART 5
Gadgets & innovations

26. WHATSAPP FOR ONLINE SUPPORT
Mobile has already taken over a huge stake of the digital market and one reason is chat apps. WhatsApp has more than
500 million monthly active users and Facebook has shown how important it thinks such platforms are by purchasing the
service for USD 19 billion earlier this year.
Created in collaboration with marketing agency CUBOCC, WhatsCook demonstrates how brands can penetrate the market
by offering a service through chat. Amateur cooks simply enter their phone number into the campaign website and arrange
a time to chat with a professional chef about a meal they need help with. As well as real-time chat, the service takes
advantage of WhatsApp’s photo and video capabilities. Users can show chefs what’s in their fridge, and chefs can take
video to demonstrate a particular technique.

27. IBOX NANO 3D PRINTER
Getting a start in 3D printing can be a pretty costly and intimidating endeavor, with most printers in the affordable
range coming in at around $1,000. But for $299, the makers of the iBox Nano aim to provide an alternative that is not
only cheaper, but also easier for novice makers to operate—so long as your 3D printing ambitions fall somewhat on the
micro side of design.
The iBox Nano is a 3D resin printer that boasts
a lot of “world’s… ,” including world’s
cheapest, lightest, smallest and quietest
3D printer and it’s also the only 3D
printer in the world that has the option
of being battery operated. While most
consumer-grade 3D printers use plastic
filament, the iBox Nano makes its creations
from a pool of resin, which is hardened layer by
layer with UV LEDs. This not only reduces the
power needs of the printer, but prevents that
icky melting plastic smell from permeating
one’s home.

28. Hope you enjoyed it.
Please keep sharing.