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SN/T 2574-2019: Determination of amitraz and metabolites residues in royal-jelly for import and export -- LC-MS/MS method Delivery: 9 seconds. True-PDF full-copy in English & invoice will be downloaded + auto-delivered via email. See step-by-step procedure Status: Valid SN/T 2574: Historical versions
Similar standardsSN/T 2574-2019: Determination of amitraz and metabolites residues in royal-jelly for import and export -- LC-MS/MS method---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/SNT2574-2019 Determination of amitraz and metabolites residues in royal-jelly for import and export - LC-MS/MS method ForewordThis standard was drafted in accordance with GB/T 1.1— 2009 “. This standard replaces SN/T 2574— 2010 Determination of amitraz and its metabolites residues in royal- jelly for import and export GC-MS. Compared with SN/T 2574— 2010, the main technical changes are as follows: —— The topic of standards was changed to “Determination of amitraz and metabolites residues in royal- jelly for export-LC-MS/MS method”. —— Delete the first method: GC-MS method. —— Increase the method: LC-MS/MS method. Please note that some of the elements of this standard may involve patents, but the standards organization does not assume responsibility for identifying these patents. This standard was proposed by and is under the charged of General Administration of Customs, of the People’ s Republic of China. This standard was drafted by Zhejiang Academy of Science and Technology for Inspection and Quarantine. The main drafters of this standard are Hou Jianbo, Xie Wen, Hong Deng, Zhang Wenhua, Sheng Tao, Mao Renyi, Wang Peng, Yan Yingpeng. This standard replaces the previous standard version: —— SN/T 2574— 2010. 1) Note: This english version, a translation from the chinese text, is solely for guidance. Determination of amitraz and its metabolites residues in royal-jelly for export —LC-MS/MS method 1 Scope This standard specifies the method for determination of amitraz, N-2, 4-dimethylphenyl-N-methylformamidine, N- (2, 4-dimethylphenyl) formamide and 2, 4-dimethyl aniline residues in royal jelly by high performance liquid chromatography tandem mass spectrometry (LC-MS/MS). This standard is applicable to determination and confirmation of amitraz, N-2, 4-dimethyl phenyl-N- methylformamidine, N- (2, 4-dimethylphenyl) formamide and 2, 4-dimethyl aniline residues in royal jelly. 2 Normative references Following documents are necessary for this standard. For dated references, only dated editions shall apply to this standard. For undated references, the latest edition of the normative document referred to applies. GB/T 6682 Water for analysis Laboratory usr— Spe cification and test methods 3 Summary The residues are extracted with ammonia acetonitrile from royal jelly sample, then the extract is cleaned up by N-Al2O3 solid phase extraction column. The residues are determined by LC-MS/MS and quantified by internal standard method [amitraz, N-2, 4-dimethyl phenyl-N-methylformamidine and 2, 4-dimethyl aniline] and external standard method [N-(2, 4-dimethylphenyl)formamide]. 4 Reagents and Materials Unless otherwise specified, all reagents used should be analytical reagent grade. “Water” is first— grade water prescribed by GB/T 6682. 4.1 Acetonitrile: HPLC grade. 4.2 Formic acid: HPLC grade. 4.3 Ammonia : 25%~28%, analytical grade. 4.4 5% ammonia solution : dilute 5 mL ammonia (4.3) to 100 mL with water. 4.5 5% ammonia of acetonitrile solution : dilute 5 mL ammonia (4.3) to 100 mL with acetonitrile(4.1). 4.6 0.15% formic acid solution : dilute 1.5 mL formic acid (4.2) to 1 000 mL with water. 4.7 Amitraz: C19H23N3, CAS No. 33089-61-1, purity ＞ 99.0%. 4.8 2, 4-dimethyl aniline ( C8H11N, CAS No: 95-68-1) purity >99.0%. 4.9 N-2, 4-dimethyl phenyl-N-methylformamidine(DMPF) (C10H14N2, CAS No: 33089-74-6): purity ＞ 99.0%. 4.10 N-(2, 4-DiMethylphenyl) formamide (DMF) (C9H11NO, CAS No: 60397-77-5) purity ＞ 99.0%. 4.11 Amitraz-D6 (C19H17D6N3) purity ＞ 99.0%. 4.12 2, 4-dimethylaniline-D6 (C8H5D6N): purity ＞ 99.0%. 4.13 Standard stock solution of amitraz: accurately weigh lomg amitraz (4.7) and dissolve with acetonitrile(4.1) to prepare standard stock solutions of 100 μg/mL. It should be stored in brown volumtric flask at 0℃～ 4℃ for 4 weeks. 4.14 Standard stock solution of 2, 4-dimethyl aniline: accurately weigh /omg 2, 4-Dimethyl aniline standards(4.8) and dissolve with acetonitrile(4.1) to prepare standard stock solutions of 100 μg/mL. It should be stored in brown volumtric flask at 0℃～ 4℃ for 4 weeks. 4.15 Standard stock solution of DMPF: accurately weigh /omg DMPF (4.9) and dissolve with acetonitrile(4.1) to prepare standard stock solutions of 100 μg/mL. It should be stored in brown volumtric flask at 0℃～ 4℃ for 4 weeks. 4.16 Standard stock solution of DMF: accurately weigh DMF /omg and dissolve with acetonitrile(4.1) to prepare standard stock solutions of 100 μg/mL. It should be stored in brown volumtric flask at 0℃～ 4℃ for 1 weeks. 4.17 Standard stock solution of Amitraz-D6: accurately weigh /omg of Amitraz-D6 (4.11) and dissolve with acetonitrile(4.1) to prepare standard stock solutions of 100 μg/mL. It should be stored in brown volumtric flask at 0℃～ 4℃ . 4.18 Standard stock solution of 2, 4-dimethylaniline-D6: accurately weigh /omg of 2, 4-dimethylaniline-D6 standards(4.12) and dissolve with acetonitrile(4.1) to prepare standard stock solutions of 100 μg/mL. It should be stored in brown volumtric flask at 0℃～ 4℃ . 4.19 Intermediate working solution: according to the concentration required, pipette appropriate volume of the above standard stock solutions and dilute to proposed working solution with acetonitrile (4.1) 4.20 N-Al2O3 solid-phase extraction (SPE) column: 1 g, 3 mL or equivalent, It should be conditioned with 3 mL acetonitrile followed by 3 mL 5% ammonia of acetonitrile solution(4.5). 4.21 Membrane filter: 0.22 μm, organic type. 5 Apparatus and equipment 5.1 Liquid chromatography-tandem mass spectrometry: equipped with electrospray ionization source (ESI). 5.2 Vortex mixer. 5.3 Centrifuge: 10 000 r/min. 5.4 Analytical balances: accuracy 0.01 g and 0.1 mg. 5.5 Nitrogen blowing instrument. 5.6 Stoppered centrifuge tube: 15 mL and 50 mL. 6 Sample preparation and storage Take appropriately 500 g of representative sample, mixed thoroughly. Then the homogenized sample is placed in a clean container as the test sample, which is sealed and labeled. Keep the prepared sample into two sample bottles, seal and label. The rest sample is stored at -18℃ in refrigerator. In the course of sample preparation, precautions should be taken to avoid contamination or any factors which may cause the change of residue content. 7 Analysis procedure 7.1 Extraction Weigh 2 g test sample (accurate to 0.01g) into a 50 mL centrifuge tube. Add internal standard solution (200 μL, 100 ng/mL). Add 8 mL 5% ammonia solution(4.4), vortex for 1 min under 2 000 r/min, wait for 5 min, add 10 mL 5% ammonia of acetonitrile solution(4.5), vortex for 1 min under 2 000 r/min, wait for 5 min, add 5% ammonia of acetonitrile solution(4.5) until total volume is 20 mL. Centrifuge for 5 min under 8 500 r/min. Transfer 2.0 mL supernatant layer into a container. Add 2 mL 5% ammonia of acetonitrile solution(4.5), mix it, centrifuge for 5 min under 8 500 r/min. Collect the supernatant to clean up. 7.2 Clean up Transfer the solution into N-Al2O3 solid-phase extraction (SPE) column (4.20), collect the eluate. Add 2 mL 5% ammonia of acetonitrile solution (4.5) elute the column deeply. The solution is evaporated to below 0.5 mL in a water bath below 40℃ to dryness. The residues was reconstituted in 2.0 mL acetonitrile and 2.0 mL water, mix it. The solution is passed through a 0.22 μm filter (4.21). The filtrate is ready for LC-MS/MS determination. 7.3 Determination 7.3.1 HPLC operating condition 7.3.1.1 LC column: C18, 150 mm × 4.6 mm (i.d.), 5μm, or equivalent column. 7.3.1.2 Injector volumn: 10 μL. 7.3.1.3 Column : 25 ℃ . ......Source: Above contents are excerpted from the full-copy PDF -- translated/reviewed by: www.ChineseStandard.net / Wayne Zheng et al. |