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SN/T 2316-2019 PDF English

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SN/T 2316-2019: Determination of p-arsanilic acid, 4-nitrophenylarsonic acid, 3-nitro-4-hydroxy-phenylarsonic acid residues in animal foods for export
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SN/T 2316: Historical versions

Standard IDUSDBUY PDFDeliveryStandard Title (Description)Status
SN/T 2316-2019235 Add to Cart Auto, 9 seconds. Determination of p-arsanilic acid, 4-nitrophenylarsonic acid, 3-nitro-4-hydroxy-phenylarsonic acid residues in animal foods for export Valid
SN/T 2316-2009639 Add to Cart 3 days Determination of p-arsanilic acid, 4-nitrophenylarsonic acid, 3-nitro-4-hydroxy-phenylarsonic acid residues in foods of animal origin. LC-ICP/MS method Obsolete

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GB 2721   GB 2711   SN/T 1888.4   SN/T 5640   

SN/T 2316-2019: Determination of p-arsanilic acid, 4-nitrophenylarsonic acid, 3-nitro-4-hydroxy-phenylarsonic acid residues in animal foods for export


---This is an excerpt. Full copy of true-PDF in English version (including equations, symbols, images, flow-chart, tables, and figures etc.), auto-downloaded/delivered in 9 seconds, can be purchased online: https://www.ChineseStandard.net/PDF.aspx/SNT2316-2019
Determination of p-arsanilic acid, 4-nitrophenylarsonic acid, 3-nitro- 4-hydroxy-phenylarsonic acid residues in animal foods for export

Foreword

This standard was drafted in accordance with GB/T 1.1— 2009. This standard was instead of SN/T 2316—2009 “Determination of p-arsanilic acid, 4-nitrophenylarsonic acid, 3-nitro-4-hydroxy-phenylarsonic acid residues in animal foods LC-ICP/MS”. This standard compares with SN/T 2316— 2009, main technology changes as follows: — The title of the standard was changed to “Determination of p-arsanilic acid, 4-nitrophenylarsonic acid, 3-nitro-4-hydroxy-phenylarsonic acid residues in animal foods for export”; — Liquid Chromatography Atomic Fluorescence Spectrometry (LC-AFS) was added as the second method. This standard was proposed by and is under the charge of General Administration of Customs of the P.R.C. This standard was drafted by Animal, Plant and Food Inspection Center of Tianjin Customs of the P.R.C., Hefei Customs of the P.R.C, Beijing Haiguang Instrument Co. Ltd and Sineo Microwave Chemistry Technology Co. Ltd. The main drafters of this standard are Xiao Yabing, Dong Zhizhen, Gao Jianhui, Han Fang, Song Wei, Ma Xing, Song Xu, Yang Shuang, Lu Yufeng and Xu Yuan. This standard replaced the following standards: — SN/T 2316— 2009. Determination of p-arsanilic acid, 4-nitrophenylarsonic acid, 3-nitro-4-hydroxy-phenylarsonic acid residues in animal foods for export

1 Scope

This standard specifies the methods of determination of p-arsanilic acid, 4-nitrophenylarsonic acid, 3-nitro-4-hydroxy-phenylarsonic acid residues by LC-ICP/MS and LC-AFS in animal foods for export which indudes principle,reagents and materials,apparatns and epumant sample preparootion and storape,proedure;callation and expression of the resulf. This standard is applicable to the determination of p-arsanilic acid, 4-nitrophenylarsonic acid, 3-nitro-4-hydroxy-phenylarsonic acid residues in chicken, chicken liver, chicken kidney, chicken offal, pork, pig liver, pig kidney and pig offal.

2 Normative reference

The following documents are essential for this document. for dated reference only dated edtions sball spply to this siardarel. For Any undated reference the latest edition (including all modifications) refend to applics. GB/T 6682 Water for analytical laboratory use-Specification and test methods. Approach 1 Liquid chromatography inductively coupled plasma / mass spectrometry

3 Principle

The p-arsanilic acid, 4-nitrophenylarsonic acid, 3-nitro-4-hydroxy-phenylarsonic acid residues were extracted with methanol+H2O (1+1, v/v), centrifuged, filtrated by 0.45um filter film, then determined by HPLC-ICP/MS, calculated by comparing peak of the sample with corresponding standard peak area.

4 Reagents and materials

Unless otherwise specified, all reagents used should be analytically pure,“water” is deionized distilled Water. 4.1 Methanol: HPLC grade. 4.2 Trifluoroacetic acid: HPLC grade. 4.3 Trifluoroacetic acid (0.1%, volume fraction): Remove 1 mL accurately trifluoroacetic acid into a 1000 mL volumetric flask, constant volume. 4.4 Filter membrane: 0.45 µm, the diameter is 47 mm. 4.5 Methanol solution: methanol +H2O (1∶1, V/V). 4.6 p-Arsanilic acid standard (C6H8AsNO3 , CAS : 122453-73-0 ) : Purity ≥ 99%. 4.7 Nitrophenylarsonic acid standard (C6H6AsNO5 , CAS: 122453-73-0 ) : Purity ≥ 95%. 4.8 Nitro-4-hydroxy-phenylarsonic acid standard (C6H6AsNO6, CAS: 122453-73-0 ): Purity ≥ 97.5%. 4.9 p-Arsanilic acid standard solution: Weigh appropriate p-Arsanilic acid, dissolve in deionized distilled water and prepare a solution of 500 µg/mL as standard stock solution. Dilute the p-Arsanilic acid standard(4.6) stock solution to the required concentration as the standard working solution with deionized distilled water. 4.10 Nitrophenylarsonic acid standard solution: Weigh appropriate p-Arsanilic acid, dissolve in deionized distilled water and prepare a solution of 500 µg/mL as standard stock solution. Dilute the 4-Nitrophenylarsonic acid standard stock solution to the required concentration as the standard working solution with deionized distilled water. 4.11 Nitro-4-hydroxy-phenylarsonic acid standard solution: Weigh appropriate p-Arsanilic acid, dissolve in deionized distilled water and prepare a solution of 500 µg/mL as standard stock solution. Dilute the 3-Nitro-4 -hydroxy-phenylarsonic acid standard stock solution to the required concentration as the standard working solution with deionized distilled water. standard stock solution shall be stored at 0 ℃ ~ 4 ℃ in refrigerator. Period of validity is 12 month. Standard working solution shall be stored at 0℃~ 4℃ in refrigerator. Period of validity is 6 month.

5 Apparatus and equipment

5.1 HPLC-ICP/MS. 5.2 Homogenizer : 15 000r/min. 5.3 Centrifuge: 3 000 r/min. 5.4 Vortex mixer 5.5 Ultrapure water system. 5.6 Electronic balances: the sensitivity is 0.1 mg and 1 mg.

6 Sample preparation and storage

6.1 Sample preparation Reduce the animal original food sample of chicken, chicken liver, chicken offal, pork, pig liver, pig kidney and pig offal to ca 500g and 100g chicken kidney by quartering, mix thoroughly and divide into 2 equal portion,place in clean containers, seal and label. 6.2 storage of test sample Animal original food shall be stored below-18℃ . In the course of sample preparation, precaution must be taken to avid contamination or any factors which may cause the change of p-Arsanilic acid, 4-Nitrophenylarsonic acid, 3-Nitro-4-hydroxy-phenylarsonic acid residue content.

7 Procedure of determination

7.1 Extraction Weigh 1 g (accurate to 0.001 g) of the test sample into the microwave assisted extraction tank, adding 10 mL of Methanol solution (4.5). The extraction was carried out according to the standard operation steps of the microwave assisted extraction apparatus (for reference conditions, see annex A, table A.1). After extraction, remove the extract and cool down to room temperature. Centrifugation at 10 000 r/min for 10 min. Take 4 3SN / T 2316—2019 mL supernatant and purge the supernatant with nitrogen, and then press the methanol solution (4.5) to 2 mL. The solution was filtered by 0.45 µm organic filter membrane(4.4). The filtrate is ready for HPLC-ICP/MS determination. The blank test is performed in the same operational approach. 7.2 Determination 7.2.1 LC operating conditions 7.2.1.1 Column: SB-C18(250mm×4.60mm)5µm or equivalent. 7.2.1.2 Mobile phase: methanol-0.1% trifluoroacetic acid(10∶90, V/V). 7.2.1.3 Flow rate: 1.0mL/min. 7.2.1.4 Injection volumn:20µL. 7.2.2 ICP/MS operating conditions The working conditions and measurement parameters of ICP/MS are shown in annex B . 7.2.3 HPLC-ICP/MS determination Preparation of p-arsanilic acid, 4-nitrophenylarsonic acid, 3-nitro-4-hydroxy-phenylarsonic acid standard solution 0.0 ug/L, 0.4 ug/L, 2.0 ug/L, 10.0 ug/L, 25.0 ug/L, 50.0 ug/L, 100.0 ug/L. The peak area is measured and the linear regression equation of the relationship between peak area and concentration is obtained. HPLC-ICP/MS spectrometry of p-arsanilic acid, 4-nitrophenylarsonic acid, 3-nitro-4-hydroxy- phenylarsonic acid standard solution (25 µg/L) see annex C. 7.2.4 Blank test The operation of the blank test is the same as that described in the method of determination but without addition of the sample. ......

Source: Above contents are excerpted from the full-copy PDF -- translated/reviewed by: www.ChineseStandard.net / Wayne Zheng et al.

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