The Advantages of Mass Detection for the Food Testing Laboratory - Waters Corporation Food Safety & QC

©2015 Waters Corporation 1
ACQUITY QDa Detector:
Accessible Mass Detection for
Food Testing

Food Industry
Challenges
 Raw Material / Ingredient Quality
– Quality needs to be as consistent as possible
– Safe
– Discrepancies may need troubleshooting / further investigation
 Final Product
– Safe
– Reformulation (low salt / sugar / functional ingredients…) can
sometimes cause analytical challenges
o New compounds need to be added to a method
• May lead to chromatographic / detector issues
 Confidence in Testing
– High demand for simple, repeatable, reliable testing techniques
in easy and complex food samples
– Need confidence in:
• Instrument used
• Results produced
Raw
Materials
In-process
production
Final
Product

Accessible & Usable
Improve Productivity
Factors influencing
Technology Adoption?
Increase Capability
Fit for Purpose

Accessible & Usable
Factors influencing
Fit for Purpose
Increase Capability

QDa
PDA
ACQUITY H-Class and QDa
With Empower 3 Software
 Simply power on and its ready to go
– Push button, fast warm up, run
samples – it just works
 Zero user set-up optimisation,
calibration or adjustments
– No sample-specific or user
adjustments typical of traditional MS
 Finished? Just power off
 Small, modular footprint
“If you can use a PDA,
you can use a QDa”
H-Class
System

Accessible & Usable
Factors influencing
Increase Capability
Fit for Purpose

ACQUITY UPLC H-Class
Analytical benefits compared to HPLC
 Enhanced analytical performance
– Greater resolution, throughput &
sensitivity
– Increase lab productivity
 Improve peak resolution
– Less co-eluting peaks
– More accurate integration ->
better RSDs
 Document no. of injections on
each column
– ACQUITY UPLC
Columns have eCords
UltraPerformance LC (UPLC)

ACQUITY UPLC H-Class
Quaternary solvent manager (QSM)
— One pump, one proportioning valve
— Continuous blending of 4 solvents
Sample manager (SM-FTN)
— “Flow-through-needle” design
— One single injection mode
Column ovens (CH-A)
— Active pre-heating
— Reduced volume to minimise extra
column band-spreading
Compatible with all ACQUITY detectors

ACQUITY UPLC
Fruit Juice Analysis
65 mins injection-to-injection;
22 samples per day

ACQUITY UPLC
Fruit Juice Analysis
Reduced run-time whilst still maintaining good resolution
15 mins injection-to-injection;
96 samples per day

Food Preservatives
HPLC conditions
0.125mg/L
15min
0.00045AU

Food Preservatives
UPLC conditions
3min
0.0045AU
10X↑
5X↑
0.125mg/L

Advantages of using
ACQUITY QDa Detector
 Compatible with Alliance & ACQUITY
 Increase sample throughput
 Highly Selective
 High Sensitivity
 Supports method development

Why Mass Detection with the
ACQUITY QDa Detector?
Detector concept
Adjustment-free & pre-optimized
Automated calibration
Familiar software
Easy to set up - can be up and
running within a very short space
of time run the samples
Ease of use and maintenance,
especially for new users
The push-button simplicity is
proven to remove the obstacles to
introducing MS data into
chromatography labs
Ease of qualitative & quantitative
data interpretation
Better accuracy, better
reproducibility, faster
turnaround for our clients

Independent Recognition
ACQUITY QDa Detector
World of Laboratory
winner for innovation
2014
PittCon Editors’ Silver Award
for Most Innovative Product
The Analytical Scientist Innovation
Awards (TASIA) 2013

Nutritional Composition
Polyphenolics for Food Quality

Application Overview
Traditional Assay Characteristics include
 Long run-times:
– Throughput limitation: problematic
 Complex ingredient profile:
– Separation & resolution; difficult
ACQUITY UPLC H-Class & ACQUITY QDa Detector
 Provides increased selectivity for compounds
of interest
– No need to get chromatographic separation
 Significantly improves analytical throughput

Beverage analysis
Polyphenolics
p-Coumaric acid
Molecular formula = C9H8O3
Molecular mass =164
Analysed [M-H]- = 163

What are SIRs?
Selected Ion Recording
 More selective and sensitive way of looking at the data on the
QDa (rather than using full scan)
 Full scan mode, e.g. 100-800 m/z
– (similar to using the setting of 190-800 nm on a eλ PDA detector)
 SIR mode, e.g. 417 m/z (m/z = mass-to-charge ratio)
– (much more selective than using e.g. 320 nm on a UV detector:
generally related to compound mass)
169
195
417
153 123….
417
m/z
100 120 140 160 180 200 220 240 260 280 300 320 340 360 380 400 420 440 460
%
0
100
255
439
417
256
m/z
100 120 140 160 180 200 220 240 260 280 300 320 340 360 380 400 420 440 460
%
0
100
255
439
417
256

Polyphenols UV v. QDa SIR
Time
3.00 3.50 4.00 4.50 5.00 5.50
0.0
1.0e-2
2.0e-2
3.0e-2
ico_Sep 16_050 (1) PDA Ch3 325nm@4.8nm
Range: 4e-2
Time
3.00 3.50 4.00 4.50 5.00 5.50
%
-10
90
Pepsico_Sep 16_050 7: SIR of 1 Channel ES+
595.3 (Didymin)
1.56e7
A
B
C
D
E
F G H
A B
C
D
E
F G
H
UV (325nm)
QDa SIR
Polyphenol m/z
A Narirutin 581.2
B Diosmin 609.2
C Hesperidin 611.2
D Didymin 595.3
E Sinensetin 373.1
F Nobiletin 403.2
G Tetramethoxyscutellarein 343.1
H Tangeretin 373.1

Polyphenols UV v. QDa SIR
Time
3.00 3.50 4.00 4.50 5.00 5.50
%
-10
90
Pepsico_Sep 16_050 7: SIR of 1 Channel ES+
595.3 (Didymin)
1.56e7
A
B
C
D
E
F G
HQDa SIR
Polyphenol m/z
F Nobiletin 403.2
G Tetramethoxyscutellarein 343.1

Analysis of flavonoids in citrus juice
(n=10)
Analyte
RT
(min)
%
Accuracy
Repeatability
(% RSD)
Narirutin 2.73 86 3
Diosmin 2.81 139 8
Hesperidin 2.87 82 3
Didymin 3.39 94 4
Sinensetin 4.36 103 4
Nobiletin 4.68 110 3
Tetramethoxyscutellarein 4.71 100 3
Tangeretin 5.02 112 3

Nutritional Composition
Non-Nutritive Sweeteners in Food & Beverages

 Variety of sweeteners are used
in sugar- free products
– Traditionally detected by multiple
optical detectors (including ELSD
and fluorescence)
Sweeteners in food & beverages
Rebaudioside A
(RebA)
Acesulfame K
Saccharin
Cyclamate
Sucralose
Stevioside
Neotame

Saccharin
Ace K
Aspartame
Neotame
AU
QDa
SIRs
PDA
Data

AU
Cyclamate
UV
transparent
Sucralose
UV
transparent
QDa
SIRs
PDA
Data

Stevioside
Reb A
Co-elution
AU
QDa
SIRs
PDA
Data

Saccharin
Ace K
Aspartame
Neotame
Stevioside
Reb A
Co-elution
AU
Cyclamate
UV
transparent
Sucralose
UV
transparent
QDa
SIRs
PDA
Data

Sucralose
UV transparent
MS Sucralose
SIR transition
UV 214nm
Sweetened with Sucralose
Sample preparation
• 1.0g mixed with 10 mL H2O
• Sonicated, shaken, centrifuged
• Inject supernatant
Quantitation of sweeteners
in Diet Marmalade

Acesulfame K
Conc ≡ 53 mg/L in tea
Sucralose
Conc ≡ 108 mg/L in tea
Permitted level = 350 mg/L
Permitted level = 400 mg/L
 Diet tea sweetened with acesulfame K and sucralose
− Sample preparation: dilution of tea in water
Quantitation of sweeteners

Regulated mycotoxins
12 regulated mycotoxins in processed maize and corn
Collaboration with Veronica Lattanzio ISPA CNR, Bari, Italy

1.NIV
2.DON
3.AFG2
4.AFG1
5.AFB2
6.AFB1
8. FB1
9. T-2
10. OTA
11. ZEA
12. FB2
Mycotoxin
Spiked
concentration
(μg kg-1)
S:N
NIV 750 1,188
DON 750 20,955
AFG2 1 5,149
AFG1 1 18,272
AFB2 1 1,967
AFB1 2 12,766
HT2 50 430
FB1 800 2,682
T-2 50 64,641
OTA 3 993
ZEA 100 6,682
FB2 200 1,967
7. HT-2
EU Permitted Limits: in Wheat
SIR Chromatograms

Example linearity in processed corn
Compound name: AFB1
Correlation coefficient: r = 0.998746, r^2 = 0.997494
Calibration curve: 764.675 * x + 22.6578
Response type: External Std, Area
Curve type: Linear, Origin: Exclude, Weighting: 1/x, Axis trans: None
3
-0.0 2.0 4.0 6.0 8.0 10.0 12.0 14.0
Response
-0
5000
10000
3
Residual
-5.0
0.0
Compound name: AFG1
Calibration curve: 398.47 * x + -57.5865
Conc
-0.00 1.00 2.00 3.00 4.00 5.00 6.00 7.00
Response
-0
1000
2000
Conc
Residual
-5.0
0.0
5.0
Compound name: T2 + NH4
Conc
-0 25 50 75 100 125 150 175 200 225 250 275 300 325 350 375
Response
-0
50000
100000
Conc
Residual
-0.00
5.00
Compound name: DON
Conc
-0 500 1000 1500 2000 2500 3000 3500 4000 4500 5000 5500
Response
-0
100000
200000
Conc
Residual
-2.50
0.00
2.50

Multiple User Interfaces
 Everyone in the lab - scientists, lab managers, system
administrators - experienced and/or new users - can easily
learn and use Empower Software to run samples, acquire and
process data, generate results from any computer using an
interface to fit their type of work.
Respond to Diverse Needs

Automated Calculations

Example Custom Fields
Suitability Acceptance

Find Data easily with View Filters

Empower 3 Network Analytics
System Analysis

Summary
 System solution is designed to be fit for
purpose
– Automated steps throughout the process from set-up
to data storage
 Improve Productivity and Lab Capacity
– Able to reduce run-times:
– Ultraperformance chromatography (UPLC)
– ACQUITY QDa selectivity
– Easy to search data within Empower
 Increase Confidence in analytical results
– Reduces chromatographic interferences
– Chromatographic interpretation is simplified

www.waters.com
Thank you for your attention

The Advantages of Mass Detection for the Food Testing Laboratory - Waters Corporation Food Safety & QC

Recommended

Recommended

More Related Content

What's hot

What's hot (20)

Viewers also liked

Viewers also liked (19)

Similar to The Advantages of Mass Detection for the Food Testing Laboratory - Waters Corporation Food Safety & QC

Similar to The Advantages of Mass Detection for the Food Testing Laboratory - Waters Corporation Food Safety & QC (20)

Recently uploaded

Recently uploaded (20)

The Advantages of Mass Detection for the Food Testing Laboratory - Waters Corporation Food Safety & QC