GB/T 19426-2006 PDF English
US$640.00 · In stock · Download in 9 secondsGB/T 19426-2006: Method for the determination of 497 pesticides and related chemicals residues in honey fruit juice and wine -- GC-MS method Delivery: 9 seconds. True-PDF full-copy in English & invoice will be downloaded + auto-delivered via email. See step-by-step procedureStatus: Obsolete GB/T 19426: Evolution and historical versions
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| GB/T 19426-2006 | English | 640 |
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Method for the determination of 497 pesticides and related chemicals residues in honey fruit juice and wine -- GC-MS method
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| GB/T 19426-2003 | English | RFQ |
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Method for the Determination of 304 Pesticides Residues in Honey, Fruit Juice and Wine -- GC-MS and LC-MS-MS detection method
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GB/T 19426-2006: Method for the determination of 497 pesticides and related chemicals residues in honey fruit juice and wine -- GC-MS method
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GB
NATIONAL STANDARD OF THE
PEOPLE’S REPUBLIC OF CHINA
ICS 67.050
X 04
Partially Replacing GB/T 19426-2003
Method for Determination of 497 Pesticides and
Related Chemicals Residues in Honey, Fruit
juice, and Wine – GC-MS Method
Issued on: DECEMBER 31, 2006
Implemented on: MARCH 1, 2007
Issued by. General Administration of Quality Supervision, Inspection and
Quarantine;
Standardization Administration of the PRC.
3. No action is required - Full-copy of this standard will be automatically &
immediately delivered to your EMAIL address in 0~60 minutes.
Table of Contents
Foreword...3
1 Scope... 4
2 Normative References...4
3 Principles... 5
4 Reagents and Materials... 5
5 Apparatus... 6
6 Preparation and Storage of Specimen... 7
7 Test Procedures...7
8 Result Calculation... 9
9 Precision...10
Appendix A...11
Appendix B...26
Appendix C...42
Appendix D...48
Appendix E...53
Appendix F... 68
Foreword
This Standard revised GB/T 19426-2003 Method for the Determination of 304
Pesticides Residues in Honey, Fruit Juice and Wine - GC-MS and LC-MS-MS.
The major revised contents include.
- Pesticides can be determined by GC-MS Method are expanded from 289 to 497
types;
- Separate LC-MS-MS Method from this Standard, and revise it into GB/T
20771-2006;
- Modify the standard name.
This Standard replaced the contents about GC-MS Method in GB/T19426-2003.
This Standard’s Appendix A, B, C, D, E and F are informative appendixes.
This Standard was proposed by Qinhuangdao Entry-Exit Inspection and Quarantine
Bureau of the People’s Republic of China.
This Standard shall be under the jurisdiction of General Administration of Quality
Supervision, Inspection and Quarantine of the People's Republic of China.
Drafting organizations of this Standard. Qinhuangdao Entry-Exit Inspection and
Quarantine Bureau of the People’s Republic of China.
Chief drafting staffs of this Standard. Pang Guofang, Fan Chunlin, Liu Yongming, Cao
Yanzhong, Zhang Jinjie, Fu Baolian, Jia Guangquan, Li Xuemin, and Wu Yanping.
The original standard was first-time issued in 2003; this Standard, together with GB/T
20771-2006, jointly replaced GB/T 19426-2003.
Method for Determination of 497 Pesticides and
Related Chemicals Residues in Honey, Fruit
juice, and Wine – GC-MS Method
1 Scope
This Standard specifies the method for determination of 497 pesticides and related
chemicals (see Appendix A) residues in honey, fruit juice and wine by GC-MS Method.
This Standard is applicable to the determination of 497 pesticides and related
chemicals residues in honey, fruit juice and wine.
This Standard’s limit of detection. 0.001 mg/kg ~ 0.300 mg/kg (see Appendix A).
2 Normative References
The provisions in following documents become the provisions of this Standard
through reference in this Standard. For dated references, the subsequent
amendments (excluding corrigendum) or revisions do not apply to this Standard,
however, parties who reach an agreement based on this Standard are encouraged to
study if the latest versions of these documents are applicable. For undated references,
the latest edition of the referenced document applies.
GB/T 6379.1 Accuracy (Trueness and Precision) of Measurement Methods and
Results - Part 1. General Principles and Definitions (GB/T 6379.1-2004, ISO
5725-1.1994, IDT)
GB/T 6379.2 Accuracy (Trueness and Precision) of Measurement Methods and
Results - Part 2. Basic Method for the Determination of Repeatability and
Reproducibility of a Standard Measurement Method (GB/T 6379.2-2004, ISO
5725-2.1994, IDT)
GB/T 6682 Water for Analytical Laboratory Use - Specification and Test Methods
(GB/T 6682-1992, neq ISO 3696.1987)
6 Preparation and Storage of Specimen
6.1 Preparation of specimen
For the non-crystallization honey sample, mix it evenly. For the crystallization honey
sample, under the sealing condition, place it in water not exceeding 60°C to gently
heat, vibrate it, after the sample is totally melted, stir it evenly; quickly cool-off to the
room temperature. Separate 0.5 kg of sample as the specimen; place it into the
sample bottle; seal, and label clearly.
For fruit juice and wine sample, pour the total original sample into the clean enameled
bucket; fully stir and mix thoroughly, then keep the mixed sample into two portions
(500 mL for each portion); seal them, take as specimen, and label clearly.
6.2 Storage of specimen
Store the specimen under the room temperature.
7 Test Procedures
7.1 Extraction
Weigh 15 g of specimen (accurate to 0.01 g), place it into 250 mL conical flask with
stopper; add 30 mL of water, dissolve 15 min by shaking at the 40°C shaking water
bath. Add 10 mL of acetone; then transfer the substances in the flask into 250 mL
separatory funnel. Use 40 mL of dichloromethane to wash the conical flask for several
times; pour the washings into separatory funnel, carefully emit gas, shake vigorously
for eight times; stand for layering; the lower-layer organic phase passes through the
cylindrical funnel loaded with anhydrous sodium sulfate; and collect it into 200 mL
heart-shaped bottle. Then successively add 5 mL of acetone and 40 mL of
dichloromethane into the separatory funnel, shake for 1 min, stand for layering, then
collect it. Repeat the extraction for twice, combine the extracted solution, which shall
be rotated and evaporated at 40°C water bath till the volume reaches 1 mL, then wait
for purification.
7.2 Purification
Add 2 cm high of anhydrous sodium sulfate into the Envi-Carb column; connect this
column to the top of Sep-Pak-NH2 column; and place the columns in series on the
holder of lower heart-shaped bottle. Before adding the sample, use 4 mL of
acetonitrile + toluene (3+1) to pre-wash the column; when the liquid surface reaches
the top of sodium sulfate, quickly transfer the sample extracted solution on the
purifying column; then use 3×2 mL of acetonitrile + toluene (3+1) to wash the sample
solution bottle; and transfer the washings into the column. Add 50mL reservoir on the
columns in series; use 25 mL of acetonitrile + toluene (3+1) to elute pesticides and
ions is consistent with that of the standard sample ions (if relative abundance ratio >
50%, then the allowable deviation is ± 10%; if relative abundance ratio > 20% ~ 50%,
then the allowable deviation is ± 15%; if relative abundance ratio > 10% ~ 20%, then
the allowable deviation is ± 20%; if relative abundance ratio ≤ 10%, then the allowable
deviation is ± 50%), then it can determine that there are pesticides and related
chemicals in the sample. If it can’t be confirmed, re-sampling; and confirm through the
scanning mode (with enough sensitivity) or increasing other confirmed ions method,
or applying other analytical apparatus with higher sensitivity.
7.3.3 Quantitative determination
This method applies the single ion quantitative determination of internal standard
method. The internal standard substance is heptachlor epoxide. To reduce the
influence of matrix, quantitative standard shall adopt matrix mixed standard working
solution. The concentration of standard solution is similar to that of the
to-be-measured compound. In this method, selected ion monitoring GC-MS diagram
of Group A, B, C, D and E standard substances in the honey matrix can refer to
Appendix D.
7.4 Parallel test
According to the above procedures, carry out the parallel test for the same specimen.
7.5 Blank test
It shall be carried out according to the above procedures except for weighing the
specimen.
8 Result Calculation
GC-MS determination result can be automatically calculated by the computer
according to the internal standard method, or be calculated according to Formula (1).
Where.
X - Residual amount of measured substance in the sample, mg/kg;
cs - Concentration of measured substance in the matrix standard working solution,
µg/mL;
A - Chromatographic peak area of measured substance in the sample solution;
As - Chromatographic peak area of measured substance in...
......
Source: Above contents are excerpted from the full-copy PDF -- translated/reviewed by: www.ChineseStandard.net / Wayne Zheng et al.
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