nias or ias? – issues from a laboratory view - · pdf filenias or ias? – issues...

GALAB Laboratories GmbH

Carsten Saal

NIAS or IAS? –Issues from a Laboratory view

� Introduction

� Company

� Our techniques and tests

� IAS and NIAS – general Background

� Non-target screening method

� Examples: NIAS or IAS?

Outline

2C.Saal: Waters Workshop 09.03.16 - Identification and quantification of unwanted substances in contact materials

� Founded in 1992

� New Building 2012 (Hamburg Bergedorf)for 200 employees on 4500 m2

Hamburg (Germany)Memmingen (Sales office) Izmir, Turkey (Sales office)

Our company


Hamburg

Hamburg Bergedorf (2013)

Our New Site (2014 completed)


Our Company

GALAB and its location

Hamburg 135 employees

Distribution of sales

- 50% Germany

- 30% Europe

- 20% worldwide


Our New Site

Chemical

LaboratoriesSampling and

preparation

Analyses and

evaluation

Microbiology /

Molecular biology

Sensory laboratory

administration


Our pillars

Food 60 %

Consumer goods 30 %

BioPharma 5 %

Environment 5 %


Our profile

fruits, vegetables, dried foods, tea, coffee, oil seeds,

rice, pastery, pastries, egg, eggproducts, milk, seafood, oils, cereals

Convenience food, baby food

Food

Consumer goods

personal care, food packaging, paper, card board, nonwoven, plastics, textiles, toys, consumer goods, adhesives, hotmelts, inks, coating,

pigments


Our Products

� We work with more than 500 Methods and analysemore than 5000 single substances in all kind of matrices

� Every Year more than 100 new substance are added

Allergens, Drug Residues, Assays, Dioxins, Elements, Endocrine Disruptors, Genetic Modified Organismn (GMO), Migration, Microbiology, MOAH, MOSH, Nonylphenols, Pesticides, Physical Testings, Product-Specifications, Protein Separation, Raw Materials, Residues, Radioactivity, Heavy Metals, SVHC, Toxins, Tributyltin, Contaminants, Packaging, Flame retardants, Phthalates, PAA, Non Target Screening


Some impressions of the Lab…


Our Team – Our State-of-the-art EquipmentAnalysis with Highest Sensitivity

Technical equipment: LC-MS/MS


Our Team – Our State-of-the-art EquipmentAnalysis with Highest Sensitivity

Technical equipment: GC-MS/MS


Project (BMEL): FOODOMICS

„Non-Targeted Metabolom-Analysis by highresolutiontime-of-flight-Massspectrometry (LC-QTOF-MS) to determinethe authenticity of food“

Goals: „metabolomic profiling“

� Determination of origin- and species.

� Distinction between conventional and organic farming


QTOF-MS mit Ion Mobility


Ionen-Mobility

Possible seperation of isobaric components

He - „air resistance“

N2 - „Dipol-interactions“

15

Common Markers

Markers prominent in Long Grain

Marker Importance

Ma

rke

r C

on

fide

nce

Markers prominent in Basmati

S Plot: Basmati vs Long grain

Quelle: Cleland G, Waters Appl. Note (2015)

16

17

Background:

NIAS or IAS?

C.Saal: Waters Workshop 09.03.16 - Identification and quantification of unwanted substances in contact materials 17

Typical Limits – IAS and NIAS

0,1 % (w/w) = 1g per Kilogramm

„Not Detectable“ = 10µg/kg or 10ppb

- e.g. for substances which are not toxic evaluated(food)

ALARA = „As Low As Reasonably Achievable“

- Based on radiation protection

- used for CMR substances (Cancerognic, mutagenicand toxic to reproduction)


The Supplychain – Nobody knows all about theproduct…

Packaging

supplier

Suppliers of rawmaterials:

- Paper

- Inks

- Pigments

- plastics

Food producer

Shops

Discounter

Laboratory

„intentionally used“

„not itentionally used“


20

Non-target-screening method


Non-target- or „10ppb“- screening“

Internal Standard

GC-MS TIC Chromatogramm (Mol-masses 33Da – 800 Da)

10 ppb level


Non-target screening results

Analytical data:

comment

compound Identification ( by data or SRM-method)

almost certainly compound Database, experience*

possible compound Database*

unknown Mass spectra*

*Evaluation possible if compered to IS:

“Overall measurement uncertainty”: -50%/+100% & risk of false positive/ negative


Qualifying screening results for validation andconformity for food contact

Analytical data:

- SRM or MRM methods

- retention time

- target masses

- qualifier masse(s) (ratio to target mass)

- Migration tests acc. to REG (EU) 10/2011Food simulantEU (VO) 10/2011

Abb. Example

10 % Ethanol A Honey

3% acetic acid B Vinegar

20% Ethanol C Liqueur

50% Ethanol D1 Milk

Vegetable oil D2 Pesto

modifiedPolyphenylenoxideMPPO (Tenax®)

E (e.g. Spaghetti)


24

Examples:

NIAS and IAS


Example 1 : Non target screening

Order:

- Extractive screening on a multilayer food contact material.

Procedure:

- Extraction of every layer and composite film by isooctane and 95% ethanol.

- GC-MSD screening.

Evaluation:

- Identification of peaks.

- Ratio of peak areas of composite film to single layer

PP film

(food contact layer)

nonwoven

PE film

Composite film

PU-adhesive


Result: Multilayer film

?


Identification of the unknown

- possible component:

cyclic esther which is formed by adipicacid with diethylene glycol.

- Identification by reference substance

- Quantification:

0,108 mg/dm² (migration)

0,648 mg/kg (food simulant)

Not toxic evaluated = 10 ppb criteria !?


Toxic evaluation of NIAS

- PU-Monomers are listed in REG (EU) 10/2011

- PU-adhesive is according to BFR recommendation XXVII

- acc. to (EU) Nr. 10/2011 passage 19-20: „…Reactionproducts should be

evaluated for risk assessment by the producer..“

- Result Risk assessment (Producer): Re-degration during digestion to thestarting monomers and a less bioavailibility of the cyclic esthers.

- 10ppb criteria is „not applicable“ for these NIAS


Background:

• Ortho-Phenylphenol

• No approved preservative

for strawberries (EC No. 396/2005)

• content strawberry: 0,08 mg/kg

Example 2 – Migration from packaging

Source

•Ortho-Phenylphenole,

approved preservative for paper/ board

(acc. to BfR-recommendation up to 0,01%)

•content: 10 mg/kg


Example 3: Mineral oil

MOSH(mineral oil saturated hydrocarbons):

MOAH (mineral oil aromatic hydrocarbons) (acc. to K. Grob: > 97% alkylated)

POSH (polyolefin saturated hydrocarbons) :

Oligomere aus Polyolefinen wie PE und PP


Draft Technical Guide Paper & Board Materials and Articles (April 2015):


Example 3 – mineral oil in black pepper

chainlenght fraction Black pepper A[mg/kg]

Black pepper B[mg/kg]

Guideline value/ Limit draftregulation

C10 – C16 MOSH 16 0,84 12 mg/kg

C16 – C20 MOSH 320 5,2 4 mg/kg

C20 – C35 MOSH 2870 11 2 mg/kg

C10 – C35 MOAH 1,6 8,5 0,5 mg/kg

Possible intentionally use of a mineral oil product duringproduction!


Carsten SaalCustomer Services

Consumer Products

Contact:

+49 40 36 80 77-433

[email protected]


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