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SN/T 3847-2019: Determination of benzodiazepines residues in foodstuffs for 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 3847: Historical versions
Similar standardsSN/T 3847-2019: Determination of benzodiazepines residues in foodstuffs for 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/SNT3847-2019 Determination of benzodiazepines residues in foodstuffs for export— LC-MS/MS method ForewordThis standard was drafted according to GB/T 1.1— 2009. This standard replaces SN/T 3847— 2014 Determination of benzodiazepines content in foods for— export LC- MS/MS method and SN/T 2220-2008 Determination of benzodiazepine residues in foodstuffs of animal origin for import and export— HPLC-MS/MS method. Compared with SN/T 3847-2014 and SN/T 2220 —2008, the mainly revision of this standard to be as follows : —— The standard name is modified to “Determination of benzodiazepines residues in foodstuffs for export— LC-MS/MS method ”. —— Modify the scope of application and chemical compound type. The application of SN/T 3847-2014 and SN/T 2220 — 2008 are health food and animal derived food respectively. This standard applies to the detection of benzodiazepines in health food and animal derived food, and adds the matrix of fish, chicken, eggs, milk, honey, and casing. Compared with SN/T 3847-2014, this standard adds α-Hydroxyalprazolam. Compared with SN/T 2220 —2008, this standard adds prazepam, nordiazepm, temazepam, clobazam, nitrazepam, lormetazepam, estazolam, lorazepam, clonazepam and etc. —— This standard combines SN/T 3847 — 2014 and SN/T 2220 — 2008 determination steps and makes appropriate modifications, for example, pH value of the extracted solution in SN/T 2220 — 2008 standard should be changed to 11.0. Please pay attention that some contents in this standard may refer to patents. The institution doesn’t take on the responsibility to identify these patents. This standard was proposed by and was under the charge of General Administration of Customs of the People’s Republic of China. The standard was drafted by Chongqing Customs District People’s Republic of China, Shanghai Customs District People’s Republic of China, Xiamen Customs District People’s Republic of China. This standard was mainly drafted by Li Xianliang, Xi Cunxian, Chen Niannian, Tang Baibin, Zeng Jing, Ren Shuo, Deng Xiaojun, Xu Dunming. This standard replaced the previous version of this standard as follows : —— SN/T 2220-2008 ； —— SN/T 3847-2014. Note: This English version, a translation from the Chinese text, is only for reference. Determination of benzodiazepines residues in foodstuffs for export —LC-MS/MS method 1 Scope This standard specifies the sample determination of prazepam, nordiazepm, chlordiazepoxide, temazepam, triaolam, clobazam, oxazepam, nitrazepam, flurazepam, lormetazepam, alprazolam, estazolam, lorazepam, clonazepam, flunitrazepam, diazepam, midazolam, desalkyflurazepam, N-desmethyflunitrazepam, α-hydroxymidazolam, 7-aminoflunitrazepam, 2-hydroxyethylflurazepam and α-hydroxyalprazolam content by LC-MS/MS in health foods and foodstuffs of animal origin for export. This standard is applicable to the determination and confirmation of benzodiazepines content in health foods (tablet, granule, capsule, syrup, oral liquid, etc.) and foodstuffs of animal origin (pork, liver, fish, chicken, egg, milk, honey, casing, etc.) . 2 Normative references The following document is necessary for this standard. For dated referenc, only dated editions shall apply to this standard. For undated references, the latest edition of the normative document (including subsequent amendments) referred to applies. GB/T 6628 Water for analytic laboratory use— Specification and test methods. 3 Principle The health food sample was extracted with dichloromethane-ether solution concentrated with rotary evaporator. The analyte was determined by LC-MS/MS, quantified by internal standard method. The benzodiazepine residues derived from foodstuffs of animal origin are hydrolyzed by β-glucuronidase followed by an extraction with acetic ether and isopropanol. The extract is cleaned up by cation-exchange solid phase extraction column. The analyte was determined by LC-MS/MS, quantified by internal standard method. 4 Reagents and materials Unless specified, all reagents should be of analytical grade ； “water” is the first grade water prescribed by GB/T 6682. 4.1 Methanol : HPLC grade. 4.2 Acetonitrile : HPLC grade. 4.3 Formic acid : HPLC grade. 4.4 Dichloromethane : HPLC grade. 4.5 Ammonium acetate. 4.6 Ethyl acetate. 4.7 Isopropanol. 4.8 Ether. 4.9 Acetic acid. 4.10 Anhydrous sodium sulfate : burn at 650 ℃ for 4 h, store in a closed container after cooling. 4.11 Borax(Na2B4O7·10H2O) . 4.12 Sodium hydroxide. 4.13 Hydrochloric acid : the concentration is 12 mol/L . 4.14 Ammonia : the concentration is 28 % . 4.15 β-glucuronidase : active of ≥ 100 000 unit/mL . 4.16 Ammonium acetate buffer : 0.02 mol/L, pH=5.2. Dissolved 1.54 g ammonium acetate (4.5) in 900 mL water, adjust pH to 5.2±0.1 with acetic acid (4.9) and add water to final volume of 1 L. The solution store at 4 ℃, assign a shelflife of 1 month. 4.17 2 mol/L sodium hydroxide solution : dissolved 8 g sodium hydroxide(4.12)in 90 mL water, add water to final volume of 100 mL after cooling. 4.18 Borax-sodium hydroxide solution : dissolved 7.6 g borax(4.11) in 900 mL water, adjust pH to 11.0±0.1 with 2 mol/L sodium hydroxide solution(4.17), diluted to the volume of 1 L. 4.19 Dichloromethane-ether solution : mix 200 mL dichloromethane(4.4) with 800 mL ether(4.8) to homogeneity. 4.20 Ethyl acetate-isopropanol solution : mix 1000 mL acetic ether with 200 mL isopropanol to homogeneity. 4.21 Acetonitrile solution : mix 20 mL acetonitrile(4.2) with 80 mL water to homogeneity, for current use. 4.22 0.1 mol/L HCl solution : weigh 9 mL hydrochloric acid(4.13), and dilute with water to final volume of 1 L. 4.23 Acetonitrile-ammonium hydroxide solution : mix 98 mL acetonitrile(4.2) with 2 mL ammonia solution (4.3), then mix well. Prepare it before use. 4.24 2 mmol/L ammonium acetate solution(including 0.2% formic acid): dissolved 0.154 g ammonium acetate(4.5), dissolve with appropriate water, and dilute to 1 000 mL after adding 2 mL formic acid(4.3), then mix well. 4.25 Benzodiazepines standard solution : the information of the standard chemical is list in annex A. The concentration of the standard solution of benzodiazepines are all 1.0 mg/mL in methanol(4.1), and the isotope internal standard solution are all 100.0 μg/mL in methanol(4.1). 4.26 Benzodiazepines standard intermedi-ate solution : diluted the standard chemical to the concentration of 1.0 μg/mL and 100.0 ng/mL with acetonitrile(4.2), store refrigerated at ＜ 5℃, assign a shelflife of 6 months. 4.27 Isotope intermediate standard solution : diluted the isotope intermediate standard solution to the concentration of 100.0 ng/mL with acetonitrile(4.2), store refrigerated at ＜ 5℃, assign a shelflife of 6 months. 4.28 Standard working solution : according to the requirement, accurately measure an adequate volume of benzodiazepines standard intermedi-ate solution (4.26) and isotope intermediate standard middle solution (4.27), dilute with acetonitrile solution (4.21) . The reference linear range is 1.0 ng/mL to 50.0 ng/mL, and the concentration of the internal standard is 10.0 isotope in pre mL solution. Prepare it before use. 4.29 Mixed cation-exchange solid phase extraction columns : 3 mL, 60 mg or equivalent. The column was washed with 5 mL methanol(4.1), and 5 mL water before use. 4.30 Membrane filter : 0.22 μm, organic. 5 Apparatus and equipment 5.1 High perfor mance liquid-chromatography tandem mass spectrometer : equipped with electrospray ionization source (ESI) . 5.2 Electronic balances : accurate to 0.01 g and 0.1 mg. 5.3 Ultrasonic extractor. 5.4 Vortex mixer. 5.5 Incubator. 5.6 Evaporator with nitrogen flow. 5.7 Centrifuge : not lower than 5 000 r/min. 5.8 Pulverize. 5.9 Volumetric flask : 10 mL, 50 mL, 100 mL. 5.10 Plastic centrifuge tube with cap : 50 mL. 6 Sample preparation and storage 6.1 Capsule, tablet, granule : about 100 g representative samples should be taken from all samples, and then mixed samples, grinded in a grind bowl(sugarcoat and capsule shell of capsule and tablet should be grinded in company), and put in suitable clean containers. After being sealed and labeled, the samples should be stored at room temperature. 6.2 Syrup, oral liquid : about 100g representative samples should be taken from all samples, and mixed samples, and then put in suitable clean containers. After being sealed and labeled, the samples should be stored at 4 ℃ in refrigerator. 6.3 Muscle, internal organs, casing, egg : about 500g representative samples should be taken from all samples, and then mixed to produce homogenous samples, and put in suitable clean containers. After being sealed and labeled, the samples should be stored below -18 ℃ in refrigerator. 6.4 Milk, honey : about 500g representative samples should be taken from all samples, and then mixed to produce homogenous samples, and put in suitable clean containers. After being sealed and labeled, the samples should be stored at 4 ℃ in refrigerator. 7 Analytical procedure 7.1 Extract procedure 7.1.1 Health food(capsule, tablet, granule, syrup, oral liquid) Accurately weigh 2 g of the test sample (accurate to 0.01 g) into a 50 mL centrifuge tube with cap, add 10 mL borax- sodium hydroxide solution (4.18) , adjust pH to approach to 11.0 with 2 mol/L sodium hydroxide solution(4.17), and add 100 μL Isotope intermediate standard solution (4.27), and add 20 mL dichloromethane-ether solution (4.19), mix to homogeneity and ultrasonic extraction for 10 min, vortex for 5 min, then centrifuge at 5 000 r/min for 5 min. Transfer the supernatant to a 100 mL distillation flask, the residue was extracted with 20 mL dichloromethane-ether solution(4.19) for twice, combine the supernatant to the distillation flask, and then evaporate the extract nearly to dryness on evaporator with nitrogen flow below 40 ℃. The residue is dissolved with 1.0 mL acetonitrile solution (4.21), vortex to homogeneity. After being filtrated with 0.22 μm filter and final solution is ready for analysis by LC-MS/MS. 7.1.2 Animal derived foods (pork, liver, fish, chicken, egg, milk, honey, casing) Accurately weigh 5 g of the test sample (accurate to 0.01 g) into a 50 mL centrifuge tube with cap, add 15.0 mL ammonium acetate buffer (4.16), vortex for 2 min, add 100.0 μL Isotope intermediate standard solution (4.27), and add 25μL β-glucuronidase(4.15), cover the lid, and then vortex for 2 min, followed by hydrolysis for 16 h at 37 ℃ in incutbatr. Adjust pH to approach to 11.0 with ammona(4.14) after hydrolization. Add 15 mL Ethyl acetate ether-isopropanol solution (4.20), vortex for 5 min, then centrifuge at 5 000 r/min for 5 min. Transfer the supernatant through an anhydrous sodium sulfate(4.10) column to a 250 mL distillation flask. The above mentioned procedure is repeated. Then combine the organic phase to an evaporator below 40 ℃ to nearly dryness. The residue is redissovled with 5.0 mL 0.1 mol/L HCl solution (4.22) for purification. 7.2 Clean up Load sample solution (7.1.2) to a conditioned mixed cation-exchange solid phase extraction columns (4.29) with the flow of 0.5 mL/min. Then the column was washed with 5 mL of water and then elute with 8 mL acetonitrile-ammonium hydroxide solution (4.23) . The eluates was concentrated to nearly dryness by gentle nitrogen below 40 ℃ . The residue is dissolved with 1.0 mL acetonitrile solution (4.21), vortex to homogeneity. After being filtrated with 0.22 μm filter and final solution is ready for analysis by LC-MS/MS. 7.3 Determination 7.3.1 LC-MS/MS operating conditions 7.3.1.1 LC column : C18, 150 mm ×2.0 (i.d.) mm, 5.0 μm or the equivalent. 7.3.1.2 Mobile phase : Acetonitrile(4.2), 2 mmol/L ammonium acetate solution(contain 0.2% formic acid)(4.24), the gradient program is listed as annex B table B.1. 7.3.1.3 Flow rate : 0.30 mL/min. 7.3.1.4 Column temperature : 40 ℃. 7.3.1.5 Injector volume : 30 μL. 7.3.1.6 Source : ESI. 7.3.1.7 Scan ning mode : positive mode. 7.3.1.8 Monitoring mode : multiple reaction monitoring(MRM). 7.3.1.9 MS/MS spectral parameters are listed as annex B table B.2. 7.3.2 Quantitive determination Under the same determination conditions, the variation range of the retention time for the peak of analyte in unknown sample and in the standard working solution can not be out of range of ±2.5 %. The variation range of the ion ratio between the two daughter ions for the unknown sample and the similar concentration can not be out of range of table 2. Then the corresponding analyte can be present in the sample. Under the instruments working condition(7.3.1), the retention time of the benzodiazepines were 7-Aminoflunitrazepam (8.8 min), chlordiazepoxide(9.4 min), midazolam(10.1 min), flurazepam(10.2 min), α-Hydroxymidazolam (10.5 min), α-Hydroxyalprazolam(12.7 min), N-Desmethyflunitrazepam(12.9 min), nitrazepam(13.0 min), oxazepam(13.1 min), estazolam(13.2 min), lorazepam (13.4 min), clonazepam (13.5 min), 2-Hydroxyethylflurazepam (13.5 min), alprazolam (13.7 min), triaolam (13.9 min), desalkyflurazepam (14.1 min), nordiazepm (14.2 min), flunitrazepam (14.2 min), temazepam (14.4 min), clobazam (14.7 min), lormetazepam (14.9 min) , diazepam (15.8 min) and prazepam (18.4 min), the MRM chromatogram of the standard is shown as annex C. ......Source: Above contents are excerpted from the full-copy PDF -- translated/reviewed by: www.ChineseStandard.net / Wayne Zheng et al. 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