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


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-ClassSystem


Accessible & Usable



Increase Capability

Fit for Purpose


ACQUITY UPLC H-ClassAnalytical 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 UPLCFruit Juice Analysis

65 mins injection-to-injection;22 samples per day


ACQUITY UPLCFruit Juice Analysis

Reduced run-time whilst still maintaining good resolution

15 mins injection-to-injection;96 samples per day


Food PreservativesHPLC 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

http://www.google.co.uk/url?sa=i&rct=j&q=&esrc=s&frm=1&source=images&cd=&cad=rja&uact=8&docid=Z-nmvGArnUV9OM&tbnid=6soLRsCpS65riM:&ved=0CAYQjRw&url=http://www.healthcareglobal.com/administration/fruit-juice-is-not-one-of-your-five-a-day&ei=TTQwU6ecIsi00QWx2oHQCw&bvm=bv.62922401,d.ZG4&psig=AFQjCNE-BHmjg7_JXazk2c0m0D4IK6j8iw&ust=1395754436556974

http://www.google.co.uk/url?sa=i&rct=j&q=&esrc=s&frm=1&source=images&cd=&cad=rja&uact=8&docid=Z-nmvGArnUV9OM&tbnid=6soLRsCpS65riM:&ved=0CAYQjRw&url=http://www.healthcareglobal.com/administration/fruit-juice-is-not-one-of-your-five-a-day&ei=TTQwU6ecIsi00QWx2oHQCw&bvm=bv.62922401,d.ZG4&psig=AFQjCNE-BHmjg7_JXazk2c0m0D4IK6j8iw&ust=1395754436556974


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 analysisPolyphenolics

p-Coumaric acid

Molecular formula = C9H8O3

Molecular mass =164

Analysed [M-H]- = 163

http://en.wikipedia.org/wiki/File:Coumaric_acid_acsv.svg

http://en.wikipedia.org/wiki/File:Coumaric_acid_acsv.svg


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)

169195

417153 123….

417

m/z100 120 140 160 180 200 220 240 260 280 300 320 340 360 380 400 420 440 460

%

0

100255

439

417

256

m/z100 120 140 160 180 200 220 240 260 280 300 320 340 360 380 400 420 440 460

%

0

100255

439

417

256


Polyphenols UV v. QDa SIR

Time3.00 3.50 4.00 4.50 5.00 5.50

AU

0.0

1.0e-2

2.0e-2

3.0e-2

Pepsico_Sep 16_050 (1) PDA Ch3 [email protected]: 4e-2

Time3.00 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

DE

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

Time3.00 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

AB

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)

AnalyteRT

(min)%

AccuracyRepeatability

(% 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

QDaSIRs

PDA Data


Sweeteners in food & beveragesA

U

Cyclamate

UV transparent

Sucralose

UV transparent

QDaSIRs

PDA Data



Stevioside

Reb A

Co-elution

AU

QDaSIRs

PDA Data



Saccharin

Ace K

Aspartame

Neotame

Stevioside

Reb A

Co-elution

AU

Cyclamate

UV transparent

Sucralose

UV transparent

QDaSIRs

PDA Data


SucraloseUV transparent

MS SucraloseSIR transition

UV 214nm

Sweetened with Sucralose

Sample preparation • 1.0g mixed with 10 mL H2O• Sonicated, shaken, centrifuged• Inject supernatant

Quantitation of sweetenersin 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

http://www.ispa.cnr.it/

http://www.ispa.cnr.it/


1.NIV

2.DON

3.AFG2

4.AFG1

5.AFB2

6.AFB1

8. FB1

9. T-2

10. OTA

11. ZEA

12. FB2

MycotoxinSpiked

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 WheatSIR Chromatograms

http://www.google.co.uk/url?sa=i&rct=j&q=&esrc=s&frm=1&source=images&cd=&cad=rja&docid=8Kblm8rlq4t1UM&tbnid=dhCPtpmC752OuM:&ved=0CAUQjRw&url=http://www.thesleuthjournal.com/wheat-may-promote-diabetes-disturbing-gut-flora/&ei=OMboUrjME-aK0AX9yIHwAg&bvm=bv.60157871,d.ZG4&psig=AFQjCNGEsyb3TAyoLwk8YqSRNB2b17Yacg&ust=1391073179266569

http://www.google.co.uk/url?sa=i&rct=j&q=&esrc=s&frm=1&source=images&cd=&cad=rja&docid=8Kblm8rlq4t1UM&tbnid=dhCPtpmC752OuM:&ved=0CAUQjRw&url=http://www.thesleuthjournal.com/wheat-may-promote-diabetes-disturbing-gut-flora/&ei=OMboUrjME-aK0AX9yIHwAg&bvm=bv.60157871,d.ZG4&psig=AFQjCNGEsyb3TAyoLwk8YqSRNB2b17Yacg&ust=1391073179266569


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

Re

sp

on

se

-0

5000

10000

3

Re

sid

ua

l

-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

Re

sp

on

se

-0

1000

2000

Conc

Re

sid

ua

l

-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

Re

sp

on

se

-0

50000

100000

Conc

Re

sid

ua

l

-0.00

5.00

Compound name: DON





Conc-0 500 1000 1500 2000 2500 3000 3500 4000 4500 5000 5500

Re

sp

on

se

-0

100000

200000

Conc

Re

sid

ua

l

-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 FieldsSuitability Acceptance


Find Data easily with View Filters


Empower 3 Network AnalyticsSystem 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


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