1 Scope
This standard specifies the method for determination of chloropropanols in foods.
Method I in this standard is applicable to the determination of 3-monochloro-1,2-propanediol (3-MCPD) in hydrolyzed vegetable protein liquid, flavorings, sausages, cheese, fish, flour, starch, cereals and breads. Method II in this standard is applicable to the determination of monochloro substituted 3-monochloro-1,2-propanediol (3-MCPD) and 2-monochloro-1,3-propanediol (2-MCPD) and dichloro substituted 1,3-dichloro-2-propanol (1,3-DCP) and 2,3-monochloro-1-propanol (2,3-DCP) in flavorings like soy sauce, vinegar, chicken powder and oyster sauce, hydrolyzed vegetable protein liquid, sausages, instant noodle seasonings. Method III in this standard is applicable to the determination of 3-MCPD, 1,3-DCP and 2,3-DCP in soy sauce, vinegar, chicken powder, hydrolyzed vegetable protein liquid and flavorings.
In this standard, determination limit and linear range for Method I are respectively 5μg/kg and 0.005ng ~ 0.600ng. Detection limit and quantitative limit for components of chloropropanol in Method II are respectively 2.0μg/kg and 5.0μg/kg, and the linear range is 0.020ng ~ 0.500ng. For Method III, quantitative limits for 3-MCPD, 1,3-DCP and 2,3-DCP are respectively 10.0μg/kg, 5.0μg/kg and 3.0μg/kg, the linear range for 3-MCPD is 20μg/kg ~ 1375μg/kg and that for both 1,3-DCP and 2,3-DCP is 2.5μg/kg ~ 90μg/kg.
Method I Determination of 3-Monochloro-1,2-Propanediol in Foods
2 Principle
Isotope dilution technology is adopted and d5-3-monochloro-1,2-propanediol (d5-3-MCPD) is adopted for internal standard quantitative analysis. Add internal standard solution into the sample, adopt kieselguhr (ExtrelutTM20) as the adsorbent to perform column chromatography separation, elute nonpolar lipid components in the sample by way of normal hexane-ethyl ether (9+1) and 3-MCPD in the sample by way of ethyl ether, and adopt heptafluorobutyryl imidazole (HFBI) solution as the derivatization reagent. Perform quantitative analysis by way of selected ion monitoring (SIM) in mass spectrum scanning mode, and quantify with internal standard method.
3 Reagents and Materials
Foreword I
Introduction II
1 Scope 1
2 Principle 1
3 Reagents and Materials 2
4 Apparatuses 2
5 Analytical Procedures 3
6 Precision 5
7 Others 5
8 Principle 6
9 Reagents and Materials 7
10 Apparatuses 7
11 Analytical Procedures 8
12 Precision 11
13 Principle 11
14 Reagents and Materials 11
15 Apparatuses 12
16 Analytical Procedures 12
17 Precision 15
Appendix A (Informative) Mass Spectrogram and Mass Chromatogram for Test 16
Appendix B (Informative) Accuracy and Precision 23
Standard
GB/T 5009.191-2006 Determination of Chloropropanols in Foods (English Version)
1 Scope
This standard specifies the method for determination of chloropropanols in foods.
Method I in this standard is applicable to the determination of 3-monochloro-1,2-propanediol (3-MCPD) in hydrolyzed vegetable protein liquid, flavorings, sausages, cheese, fish, flour, starch, cereals and breads. Method II in this standard is applicable to the determination of monochloro substituted 3-monochloro-1,2-propanediol (3-MCPD) and 2-monochloro-1,3-propanediol (2-MCPD) and dichloro substituted 1,3-dichloro-2-propanol (1,3-DCP) and 2,3-monochloro-1-propanol (2,3-DCP) in flavorings like soy sauce, vinegar, chicken powder and oyster sauce, hydrolyzed vegetable protein liquid, sausages, instant noodle seasonings. Method III in this standard is applicable to the determination of 3-MCPD, 1,3-DCP and 2,3-DCP in soy sauce, vinegar, chicken powder, hydrolyzed vegetable protein liquid and flavorings.
In this standard, determination limit and linear range for Method I are respectively 5μg/kg and 0.005ng ~ 0.600ng. Detection limit and quantitative limit for components of chloropropanol in Method II are respectively 2.0μg/kg and 5.0μg/kg, and the linear range is 0.020ng ~ 0.500ng. For Method III, quantitative limits for 3-MCPD, 1,3-DCP and 2,3-DCP are respectively 10.0μg/kg, 5.0μg/kg and 3.0μg/kg, the linear range for 3-MCPD is 20μg/kg ~ 1375μg/kg and that for both 1,3-DCP and 2,3-DCP is 2.5μg/kg ~ 90μg/kg.
Method I Determination of 3-Monochloro-1,2-Propanediol in Foods
2 Principle
Isotope dilution technology is adopted and d5-3-monochloro-1,2-propanediol (d5-3-MCPD) is adopted for internal standard quantitative analysis. Add internal standard solution into the sample, adopt kieselguhr (ExtrelutTM20) as the adsorbent to perform column chromatography separation, elute nonpolar lipid components in the sample by way of normal hexane-ethyl ether (9+1) and 3-MCPD in the sample by way of ethyl ether, and adopt heptafluorobutyryl imidazole (HFBI) solution as the derivatization reagent. Perform quantitative analysis by way of selected ion monitoring (SIM) in mass spectrum scanning mode, and quantify with internal standard method.
3 Reagents and Materials
Contents of GB/T 5009.191-2006
Foreword I
Introduction II
1 Scope 1
2 Principle 1
3 Reagents and Materials 2
4 Apparatuses 2
5 Analytical Procedures 3
6 Precision 5
7 Others 5
8 Principle 6
9 Reagents and Materials 7
10 Apparatuses 7
11 Analytical Procedures 8
12 Precision 11
13 Principle 11
14 Reagents and Materials 11
15 Apparatuses 12
16 Analytical Procedures 12
17 Precision 15
Appendix A (Informative) Mass Spectrogram and Mass Chromatogram for Test 16
Appendix B (Informative) Accuracy and Precision 23
