Determination Of Benzoic Acid, Sorbic Acid, And Methyl, Ethyl, Propyl, And Butyl Parabens By Hplc

Páginas: 13 (3012 palabras) Publicado: 15 de mayo de 2012
United States Department of Agriculture

Food Safety and Inspection Service, Office of Public Health Science

Page 1 of 15

SOP No: CLG-BSP.01

Title: Determination of Benzoic Acid, Sorbic Acid, and Methyl, Ethyl, Propyl, and Butyl
Parabens by HPLC
Revision: .01

Replaces: Guidebook Method,
May 1993

Effective: 11-1-04

Contents
A.

INTRODUCTION....................................................................................... 2




B.

EQUIPMENT ............................................................................................. 2




C.

REAGENTS AND SOLUTIONS ................................................................ 3


D.

STANDARDS ............................................................................................4




E.

SAMPLE PREPARATION ......................................................................... 5




F.

ANALYTICAL PROCEDURE..................................................................... 5




H.

SAFETY PRECAUTIONS AND INFORMATION ....................................... 8


I.

QUALITY ASSURANCE PLAN............................................................... 10




J.

WORKSHEET ......................................................................................... 12




K.

APPENDIX .............................................................................................. 14




United States Department of Agriculture

Food Safety and Inspection Service, Office of Public Health Science

Page 2 of 15

SOPNo: CLG-BSP.01

Title: Determination of Benzoic Acid, Sorbic Acid, and Methyl, Ethyl, Propyl, and Butyl
Parabens by HPLC
Revision: .01

Replaces: Guidebook Method,
May 1993

A.

INTRODUCTION


1.

Effective: 11-1-04

Theory

The antimicrobial preservatives benzoic acid, sorbic acid, and parabens are not
permitted in fresh meat products or in seasoning mixtures used in theformulation of
these products.
Ten grams of thoroughly comminuted meat samples are extracted with 70 mL ethanol.
After filtration, extracts are analyzed by reverse phase liquid chromatography, using a
254 or 280 nm UV detector.

2.

pplicability
A
This method is applicable for meat products at levels listed in I. 1.

B.

EQUIPMENT

Note: Equivalent apparatus and instrumentation maybe substituted for any of the
following.

1.

Apparatus

a.
b.

Stirring bar - Plastic-coated, magnetic, 1" long.

c.

Filter paper - Reeve Angel grade 802, Sargent-Welch Scientific Co., Skokie, IL,
fast-filtering and medium porosity (18.5 cm).

d.

Solvent clarification kit - With Durapore filters (0.4 µm, 47 mm), but without pump
and filtering flask, WatersAssociates, Milford, MA.

e.

Evaporator - N-Evap, Model III, Organomation Associates, Inc., South Berlin,
MA.

f.

Sample filtration apparatus - Stainless steel Swinney filter holder, with 0.45 0.50 µm, Fluoropore, Nylon 66 or PTFE filters, Millipore Corp., Bedford, MA.

g.
2.

Magnetic stirrer - Variable-speed, Nuova 7 Thermolyne, Sybron Corp., Dubuque,
IA.

pH meter - FisherAccumet, Model 210, Fisher Scientific Co., Pittsburgh, PA.

Instrumentation

a.

Liquid chromatograph

i.

Waters Alliance LC system consisting of a 2690 Separations Module.

ii.

Model 996 PhotoDiode Array Detector.

iii.

Integrator or integrating software.

United States Department of Agriculture

Food Safety and Inspection Service, Office of Public Health SciencePage 3 of 15

SOP No: CLG-BSP.01

Title: Determination of Benzoic Acid, Sorbic Acid, and Methyl, Ethyl, Propyl, and Butyl
Parabens by HPLC
Revision: .01

iv.

C.

Replaces: Guidebook Method,
May 1993

Effective: 11-1-04

Column - 15cm x 4.6mm ID, Luna C-18 (2), 5 µm spherical silica
(Phenomenex).

REAGENTS AND SOLUTIONS
Note: Equivalent reagents and solutions may be...
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