1 Scope
This standard specifies the LC-MS/MS determination method for hormone residues in foodstuffs of animal origin.
This standard is applicable to the confirmation and quantitative determination for residues of 50 kinds of hormone (See Appendix A) in foodstuffs of animal origin such as pork, pork liver, egg, milk, beef, chicken and shrimp etc.
2 Normative References
The following documents contain provisions which, through reference in this text, constitute provisions of this standard. For dated references, subsequent amendments to (excluding amending error in the text), or revisions of, any of these publications do not apply. However, all parties coming to an agreement according to this standard are encouraged to study whether the latest edition of these documents is applicable. For undated references, the latest edition of the normative document is applicable to this standard.
GB/T 6682 Water for Laboratory Use-Specifications (GB/T 6682-1992, neq ISO 3696: 1987)
3 Summary of Methods
Target compound in samples is extracted by methanol -water solution after homogenizing and enzymolysis, purified after solid phase extraction and enrichment, determined by LC-MS/MS instrument and quantified by internal standard method.
4 Reagents and Materials
Unless otherwise specified, the adopted reagents in this standard are all chromatographically pure, and the water is Grade 1 water specified in GB/T 6682.
4.1 Methanol
4.2 Methylene chloride
4.3 Acetonitrile
4.4 Formic acid
4.5 Acetic acid: analytical reagent
4.6 Sodium acetate (NaAC•4H2O): analytical reagent
4.7 β-glycuronidase/arylsulfatase solution: 4.5U/mL β-glycuronidase and 14U/mL arylsulfatase.
4.8 Acetic acid-sodium acetate buffer solution (pH 5.2): 43.0g sodium acetate (NaAC•4H2O) is weighed, 22mL acetic acid is added and water is adopted to dissolve it and scale the volume to 1000mL and then acetic acid is adopted to adjust the PH to 5.2.
4.9 Methanol-water solution (1+1, volume ratio): 50mL methanol and 50mL water are fetched for the mixing.
1 Scope
2 Normative References
3 Summary of Methods
4 Reagents and Materials
5 Instruments
6 Sample Preparation
7 Analysis Procedures
8 Determination
9 Qualitation
10 Quantitation
11 Calculation
12 Determination Low Limit and Recovery Rate
Appendix A (Normative) English Names and CAS No. of 50 Kinds of Hormone Substance and Corresponding Internal Standard Substance
Appendix B (Normative) English Names of 18 Kinds of Internal Standard Substance
Appendix C (Informative) Reference LC Conditions
Appendix D (Informative) Reference MS Condtions1)
Appendix E (Informative) MRM Spectrogram of Standard Substance
Appendix F (Informative) Lower Limit for the Determination of 50 Kinds of Hormone
Appendix G (Informative) Standard Recovery Rate and Relative Standard Deviation (RSD) of Methods
1 Scope
This standard specifies the LC-MS/MS determination method for hormone residues in foodstuffs of animal origin.
This standard is applicable to the confirmation and quantitative determination for residues of 50 kinds of hormone (See Appendix A) in foodstuffs of animal origin such as pork, pork liver, egg, milk, beef, chicken and shrimp etc.
2 Normative References
The following documents contain provisions which, through reference in this text, constitute provisions of this standard. For dated references, subsequent amendments to (excluding amending error in the text), or revisions of, any of these publications do not apply. However, all parties coming to an agreement according to this standard are encouraged to study whether the latest edition of these documents is applicable. For undated references, the latest edition of the normative document is applicable to this standard.
GB/T 6682 Water for Laboratory Use-Specifications (GB/T 6682-1992, neq ISO 3696: 1987)
3 Summary of Methods
Target compound in samples is extracted by methanol -water solution after homogenizing and enzymolysis, purified after solid phase extraction and enrichment, determined by LC-MS/MS instrument and quantified by internal standard method.
4 Reagents and Materials
Unless otherwise specified, the adopted reagents in this standard are all chromatographically pure, and the water is Grade 1 water specified in GB/T 6682.
4.1 Methanol
4.2 Methylene chloride
4.3 Acetonitrile
4.4 Formic acid
4.5 Acetic acid: analytical reagent
4.6 Sodium acetate (NaAC•4H2O): analytical reagent
4.7 β-glycuronidase/arylsulfatase solution: 4.5U/mL β-glycuronidase and 14U/mL arylsulfatase.
4.8 Acetic acid-sodium acetate buffer solution (pH 5.2): 43.0g sodium acetate (NaAC•4H2O) is weighed, 22mL acetic acid is added and water is adopted to dissolve it and scale the volume to 1000mL and then acetic acid is adopted to adjust the PH to 5.2.
4.9 Methanol-water solution (1+1, volume ratio): 50mL methanol and 50mL water are fetched for the mixing.
Contents of GB/T 21981-2008
1 Scope
2 Normative References
3 Summary of Methods
4 Reagents and Materials
5 Instruments
6 Sample Preparation
7 Analysis Procedures
8 Determination
9 Qualitation
10 Quantitation
11 Calculation
12 Determination Low Limit and Recovery Rate
Appendix A (Normative) English Names and CAS No. of 50 Kinds of Hormone Substance and Corresponding Internal Standard Substance
Appendix B (Normative) English Names of 18 Kinds of Internal Standard Substance
Appendix C (Informative) Reference LC Conditions
Appendix D (Informative) Reference MS Condtions1)
Appendix E (Informative) MRM Spectrogram of Standard Substance
Appendix F (Informative) Lower Limit for the Determination of 50 Kinds of Hormone
Appendix G (Informative) Standard Recovery Rate and Relative Standard Deviation (RSD) of Methods
