Customer Focused, Science Driven, Results Led

Elemental Analysis in Infant Formulations and Dairy Products

Using MP-AES, ICP-OES and ICP-MS

Calum McOmish, Metals Laboratory Manager

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About RSSL

•We provide science and technology outsourcing to the global FMCG and pharmaceutical industries and their suppliers based from our facility in Reading

•We understand the needs, problems and issues of industry and work with you to solve your problems and support your business

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Our Expertise

We support with:

• Product & contaminant analysis• Problem solving & investigative analysis• Product development•Claim substantiation• Training & consultancy

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Techniques on Site

Extensive capability on site including:

• Chromatography techniques (HPLC, GC, UPLC, Ion)• Microscopy (XRF, FT-IR, SEM, Confocal scanning laser

microscope, X-ray tomography)

• Physical sciences (DSC, PSD, Rheometers, TGA, DVS, Texture analysers, Zetasizer)

• NMR, ELISA, PCR, AAS, ICP-OES• Mass spectroscopy (GC-MS, LC-MS, LC-TOF,

PTR-MS, ICP-MS)

Elemental Analysis of Dairy Products/Infant Formula

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Possible analytical techniques:• ICP-MS • ICP-OES• MP-AES• AAS (flame, graphite furnace & hydride/cold

vapour generation)• XRF

RSSL’s Instrumentation

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Agilent 7700 ICP-MS• Great for trace elements (sub ppb)

• Simultaneous detection

• High dilutions required for assays

• UKAS accredited for 11 elements in unspecified foods: Al, Sb, As, Ba, Cd, Cr, Co, Cu, Fe, Pb, Mn, Hg, Mo, Ni, Tl & Zn

• I being added to scope later in 2016

• 8800 ICP-MS QQQ being purchased in June to expand capacity and capability

RSSL’s Instrumentation

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Agilent 720 ICP-OES• Good for both trace analysis and assays

• Simultaneous detection

• Very fast analysis with SVS2

• Routinely used for mineral analysis

and transition metals

RSSL’s Instrumentation

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Agilent 4200 MP-AES• Great for mineral analysis

• Sequential detection

• Cheap to run

• Better sensitivity and dynamic range than AAS

• UKAS accreditation being applied for 11 elements in unspecified foods:

Na, Mg, Ca, K, P, Zn, Fe, Mn, Cr, Ni & Cu

Elemental Analysis of Dairy Products/Infant Formula

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Sample preparation:

• Heatblock digestion

With HNO3 and H2O2 (raw milk, milk powders)

• Microwave digestion (infant formula, complex dairy products)

EU Regulations – Heavy Metals

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• Commission Regulation (EC) No 1881/2006 setting maximum levels for certain contaminants in foodstuffs

Lead (Pb) Maximum level (mg/kg wet weight)

Cow’s milk (raw milk, heat-treated milk andmilk for the manufacture of milk-based products

0.020

Infant formulae and follow-on formulae 0.020

Tin (Sn) inorganic Maximum level (mg/kg wet weight)

Canned infant formulae and follow-on formulae (including infant milk and follow on milk), excluding dried and powdered products

50

Cases of Lead Poisoning in Cattle

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• 2006

England - vehicle batteries mixed with cattle feed

• 2008

Northern Ireland – car batteries dumped in corner of field

• 2014

Wales - storm water washed high levels of lead from disused lead mines onto grass which was then cut for silage

• 2016

Ireland - degrading lead weights on collars worn by cows contaminating feed

Milk Powder

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Very versatile ingredient:

• Infant formula

• Chocolate

• Seasoning mixes

• Confectionary

• Bakery goods (biscuits, cakes etc.)

• Pharmaceuticals

Due diligence testing required to ensure limits are not breeched

EU Regulations – Minerals

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• Commission Directive 2006/141/EC on infant formulae and follow-on formulae

• Infant formulae and follow-on formulae manufactured from cows’ milk

proteins or protein hydrolysates (per 100 kcal)

Mineral Min Max

Sodium (mg) 20 60

Potassium (mg) 60 160

Chloride (mg) 50 160

Calcium (mg) 50 140

Phosphorus (mg)

25 90

Magnesium (mg) 5 15

Mineral Min Max

Iron (mg) 0.30.6

1.32

Zinc (mg) 0.5 1.5

Copper (µg) 35 100

Iodine (µg) 10 50

Selenium (µg) 1 9

Manganese (µg) 1 100

Fluoride (µg) - 100

• The Ca:P ratio in infant formulae and follow-on formulae shall not be less than

1 nor greater than 2

Minerals in Skimmed Milk Powder

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• Comparison of skimmed milk powder from two different manufacturers

• Samples Analysed for Na, Mg, Ca, K and P using both MP-AES (4200) and ICP-OES (720) – results in mg/kg

Sample Technique Na Mg Ca K P

SMP1 MP-AES 13412 1210 8629 17065 4241ICP-OES 13298 1219 8591 17157 4258%RSD 0.60 0.52 0.31 0.38 0.28

SMP2 MP-AES 9189 801 7104 9374 3398ICP-OES 9234 792 7178 9241 3444%RSD 0.35 0.80 0.73 1.01 0.95

• Results obtained between two instruments very comparable with excellent RSDs

Proficiency Testing - FAPAS

Al Cd Cr I Mo Se

Sep-13

Assigned Value x x 178 102 401 40.9

RSSL Value x x 172 91 404 43

z-Score x x -0.2 -0.5 0 0.2

Sep-14

Assigned Value 2356 x 125 1082 449 161

RSSL Value 2197 x 120 1100 400 170

z-Score -0.5 x -0.2 0.1 -0.6 0.3

Sep-15

Assigned Value 2475 14.7 248 1090 441 158

RSSL Value 2430 13.9 226 1070 445 209

z-Score -0.1 -0.3 -0.5 -0.1 0 1.5

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• Infant Formula – Tested by ICP-MS (results in µg/kg)

Questions

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Elemental Analysis in Infant Formulations and Dairy Products Using MP-AES, ICP-OES and ICP-MSAbout RSSLOur ExpertiseTechniques on SiteElemental Analysis of Dairy Products/Infant Formula�RSSL’s InstrumentationRSSL’s InstrumentationRSSL’s InstrumentationElemental Analysis of Dairy Products/Infant Formula�EU Regulations – Heavy MetalsCases of Lead Poisoning in CattleMilk Powder�EU Regulations – MineralsMinerals in Skimmed Milk PowderProficiency Testing - FAPASQuestions