LPS-004
Determination of Bisphenol A in Liquid Infant Formula
by Solid Pha Extraction with Acetic Anhydride Derivatization and Gas Chromatography–Mass Spectrometry
Bureau of Chemical Safety
Food Directorate
Health Products and Food Branch
A WHO Collaborating Centre for
齐刘海怎么剪好看
Food Contamination Monitoring
Health Canada is the federal department responsible for helping the people of Canada maintain and improve their health. We asss the safety of drugs and many consumer products, help improve the safety of food, and provide information to Canadians to help them make healthy decisions. We provide
health rvices to First Nations people and to Inuit communities. We work with the provinces to ensure our health care system rves the needs of Canadians.
Published by Authority of the Minister of Health.
LPS-004 Determination of Bisphenol A in Liquid Infant Formula by Solid Pha Extraction with Acetic Anhydride Derivatization and Gas Chromatography-Mass Spectrometry is available on Internet at the following address:
a/fn-an/res-rech/analy-meth/chem/lps_004_e.html.
Également disponible en français sous le titre :皇甫姓氏是贵族吗
LPS-004 Dosage de bisphénol A dans une préparation liquide pour nourrissons par extraction en pha solide avec une dérivatisation à l’anhydride acétique suivie d’une chromatographie en pha gazeu couplée à une spectrométrie de mas.
This publication can be made available on request on diskette, large print, audio-castte and braille.
For further information or to obtain additional copies, plea contact:
Publications
Health Canada
Ottawa , Ontario K1A 0K9
Tel.: (613) 954-5995
Fax: (613) 941-5366
E-Mail: a
© Her Majesty the Queen in Right of Canada, reprented by the Minister of Health Canada, 2008.
Cat.: H164-80/2008E-PDF
ISBN: 978-0-662-48685-5
2 |Bureau of Chemical Safety, Food Directorate, Health Products and Food Branch
TABLE OF CONTENTS
1.0PRINCIPLE AND SCOPE (4)
2.0DEFINITIONS (4)
党员工作小结
3.0PERFORMANCE CHARACTERISTICS (4)
4.0EQUIPMENT AND SUPPLIES (4)
4.1Equipment (4)
4.2Chemicals (5)
4.3Materials (5)
5.0HEALTH AND SAFETY (5)
6.0PROCEDURES (5)食品厂生产车间
6.1Preparation of Standard Solutions (5)
6.2Sample Extraction (6)
6.3Derivatization (7)
6.4Instrumental Conditions (8)
7.0QUALITY CONTROL AND QUALITY ASSURANCE (9)
8.0ASSOCIATED DOCUMENTS (9)
Bureau of Chemical Safety, Food Directorate, Health Products and Food Branch |3
1.0 Principle and Scope
This method is for determination of bisphenol-A in liquid infant formulae at levels from 0.3 to 25 ppb.
Labelled BPA-d16 is ud as internal standard. The milk proteins are denatured and
parated using acetonitrile. Fats, carbohydrates and some of the added fatty acids are
removed by SPE.
BPA is derivatized to the di-ester using acetic anhydride in basic aqueous solution. The
derivative of BPA is extracted using a non-polar solvent, and measured by GC/MS in SIM mode using 4 ions (one target and 3 qualifiers). Calibration standards are prepared the
same way as samples (from the derivation step).
2.0 Definitions
BPA: Bisphenol A
BPA-d16 : Isotopic labelled Bisphenol A-d16
ACN: Acetonitrile
Characteristics
3.0 Performance
Intra-assay
BPA levels (ng/g) Recovery (%) RSD %
2.5 (n=8) 94 2.8
方向跑偏
20.0 (n=5) 94 3.9
8.0 (n=8) 85 2.7
Inter-assay validation data
BPA
%
RSD
(%)
n ng/g Recovery
High concentration
心猿意马啥意思6 10.4 ---------- 2.8
reference material
6 0.54 ---------- 5.0
Low concentration
reference material
Method blanks 6 0.13 ---------- ----------
Spiked blanks 6 ---------- 100 1.4
Duplicates 5 1.9
4.0 Equipment and Supplies
4.1 Equipment
4.1.1 Agilent 6890 gas chromatograph with 5975 mass lective detector
4.1.2 Oven
4.1.3 Balances
4.1.4 50-position stirring plate for 22-mL vials (Barnstead # PS80037A)
bath
4.1.5 Ultrasonic
4.1.6 pH meter and calibration solutions
4.1.7 N2 evaporator 12 or 24 positions
4.1.8 Vortexes, simple and multi-tubes
4.1.9 Speedvac
evaporator system
4 |Bureau of Chemical Safety, Food Directorate, Health Products and Food Branch
4.2 Chemicals
4.2.1 Acetonitrile (HPLC grade) from J.T. Baker (Phillipsburg, N.J.).
4.2.2 Methanol (HPLC grade) from J.T. Baker (Phillipsburg, N.J.).
4.2.3 Toluene (glass distilled) from Sigma-Aldrich (Oakville, ON).
(ACS grade) from Sigma-Aldrich (Oakville, ON).
4.2.4 Potassium
carbonate
4.2.5 Bisphenol A (99%) from Sigma-Aldrich (Oakville, ON).
否定转移
4.2.6 Bisphenol A-d16 (98%) from Sigma-Aldrich (Oakville, ON).
4.2.7 Isooctane (pesticide-residue grade) from Sigma-Aldrich (Oakville, ON).
4.2.8 MTBE (methyl t-butyl ether, 99.9%) from Sigma-Aldrich (Oakville, ON).
4.2.9 K2HPO4 (ACS) from Sigma-Aldrich (Oakville, ON).
4.2.10 Na2SO4 (anhydrous, ACS grade) from Sigma-Aldrich (Oakville, ON).
4.2.11 1-Pentanol (99%), dodecane (99%) from Sigma-Aldrich (Oakville, ON).
4.2.12 Acetic anhydride (ACS grade) from Fisher (Ottawa, ON).
4.2.13 H3PO4 (85% HPLC grade) from Fisher (Ottawa, ON).
4.2.14 Deionized water from a milli-Q system.
4.3 Materials
4.3.1 15 mL polypropylene centrifuge tubes
4.3.2 Volumetric flasks, 10, 25, 50, 100 mL
4.3.3 Disposable glass tubes, 13 x 100 mm, 16 x 100 mm, 20 x 150 mm
4.3.4 2 mL autosampler amber vials
4.3.5 Stirring bars, 12.5 x 5 mm
4.3.6 22 mL vials with Teflon-coated ptum caps
4.3.7 Eppendorf pipettes, 100 – 1000 μL, 10 – 100 μL, 20 – 250 μL
4.3.8 pH indicating papers, 1 – 14
4.3.9 C18 SPE cartridges, 500 mg/6 cc from Varian (Mississauga, ON.)
4.3.10 80 mL rervoirs for SPE with adaptors
4.3.11 Vacuum manifold for SPE 20 positions
4.3.12 10 – 50 mL bottle-top dispenr
4.3.13 70 mL glass tubes with Teflon-coated ptum and screw caps
4.3.14 Empty glass column with frit.
5.0 Health and Safety
6.0 Procedures
6.1 Preparation of Standard Solutions
6.1.1 BPA stock Solutions (400 ppm): Prepare in 25 mL volumetric flask, using
acetonitrile as solvent; store at 4o C.
6.1.2 BPA Intermediate and spiking solution (10.0 ppm): In a 25 mL volumetric flask,
pipette the necessary volume of stock solution of BPA to get a concentration of
生日那天
10.0 μg/mL. Fill up with acetonitrile.
Bureau of Chemical Safety, Food Directorate, Health Products and Food Branch |5
