SFT0066-2020 English PDFUS$649.00 · In stock
Delivery: <= 5 days. True-PDF full-copy in English will be manually translated and delivered via email. SFT0066-2020: (Liquid chromatography-tandem mass spectrometry method for 31 new fentanyl psychoactive substances and their metabolites in fentanyl and other biological samples) Status: Valid
Basic dataStandard ID: SF/T 0066-2020 (SF/T0066-2020)Description (Translated English): (Liquid chromatography-tandem mass spectrometry method for 31 new fentanyl psychoactive substances and their metabolites in fentanyl and other biological samples) Sector / Industry: Chinese Industry Standard (Recommended) Classification of Chinese Standard: C06 Word Count Estimation: 28,293 Date of Issue: 2020-05-29 Date of Implementation: 2020-05-29 Regulation (derived from): Announcement of the Ministry of Justice (2020.05.29) Issuing agency(ies): Ministry of Justice of the People's Republic of China SFT0066-2020: (Liquid chromatography-tandem mass spectrometry method for 31 new fentanyl psychoactive substances and their metabolites in fentanyl and other biological samples)---This is a DRAFT version for illustration, not a final translation. Full copy of true-PDF in English version (including equations, symbols, images, flow-chart, tables, and figures etc.) will be manually/carefully translated upon your order. Determination of 31 fentanyl-analogue and their metabolites in biological samples by liquid chromatography- tandem mass spectrometry ICS 07.140 C 06 SF People's Republic of China judicial administration industry standards Fentanyl and other 31 new spirits of fentanyl in biological samples Liquid chromatography-tandem mass spectrometry of active substances and their metabolites Testing method 2020-05-29 released 2020-05-29 implementation Issued by the Ministry of Justice of the People's Republic of China Table of contentsForeword...II 1 Scope...1 2 Normative references...1 3 Terms and definitions...1 4 Principle...1 5 Reagents, instruments and materials...1 6 Operation method...3 7 Evaluation of analysis results...8 Appendix A (informative appendix) Extracted ion chromatograms of 31 new fentanyl-type psychoactive substances and their metabolites...10 Appendix B (informative appendix) Methodological validation data...17ForewordThis standard was drafted in accordance with the rules given in GB/T 1.1-2009. Please note that certain contents of this document may involve patents. The issuing agency of this document is not responsible for identifying these patents. This standard was proposed by the Forensic Science Research Institute. This standard is under the jurisdiction of the Information Center of the Ministry of Justice. Drafting organization of this standard. Forensic Forensic Science Research Institute. The main drafters of this standard. Shi Yan, Xiang Ping, Liu Wei, Shen Baohua, Yan Hui, Zhuo Xianyi, Shen Min, Wu Hejian. Fentanyl and other 31 new fentanyl psychoactive substances and their metabolites in biological samples Liquid chromatography-tandem mass spectrometry method1 ScopeThis standard specifies the liquid chromatography of 31 new fentanyl-type psychoactive substances and their metabolites in blood, urine, and hair. Tandem mass spectrometry (LC-MS/MS) inspection reagents, instruments and materials, operating methods and analysis results evaluation requirements. This standard applies to the qualitative and quantitative determination of 31 new fentanyl-type psychoactive substances and their metabolites in blood, urine and hair, including fentanyl For analysis, the qualitative and quantitative analysis of 31 new fentanyl-type psychoactive substances and their metabolites in other samples can be used as reference.2 Normative referencesThe following documents are indispensable for the application of this document. For dated reference documents, only the dated version applies to this document. For undated references, the latest version (including all amendments) applies to this document. GB/T 6682 Analytical laboratory water specifications and test methods GA/T 122 Terminology for toxicological analysis3 Terms and definitionsThe terms and definitions established in GA/T 122 apply to this document.4 PrincipleAfter the blood, urine, and hair samples are extracted by organic solvents, they are detected by liquid chromatography-tandem mass spectrometry (LC-MS/MS). The blank sample operated in parallel and the added sample were used as controls, and the retention time and relative abundance ratio of the two parent ion/product ion pairs were used for qualitative analysis. Analysis; Based on the peak area of the quantitative ion pair, the internal standard method is used for quantitative analysis. 5 Reagents, instruments and materials 5.1 Reagents The test water should be the first grade water that meets the requirements of GB/T 6682.The reagents and requirements used are as follows. a) Methanol. HPLC grade; b) Acetonitrile. HPLC grade; c) 98% formic acid. pure superior grade; d) Ammonium acetate. chromatographically pure; e) Acetone. analytically pure; f) Standard substance solution. 5.2 Apparatus and materials The equipment, materials and requirements are as follows. a) Liquid chromatography-tandem mass spectrometer. equipped with electrospray ionization source (ESI); b) Electronic analytical balance. division value 0.1mg; c) Centrifuge. the maximum relative centrifugal force is 14100×g; d) Ultrasonic cleaner; e) Centrifuge tube and grinding tube; f) Filter membrane. 0.22μm; g) Freezing grinder; h) Micropipette.6 Operation method6.1 Qualitative analysis 6.1.1 Sample preparation 6.1.1.1 Case samples 6.1.1.1.1 Body fluid samples Take 100μL of whole blood or urine, accurately add 10μL of 100ng/mL internal standard working solution, mix for 10s, add borax buffer solution (pH9.2) 100μL, 0.7mL ethyl acetate, vortex for 30s, centrifuge at 9700×g for 5min. Take the upper organic phase and place it in a 5mL centrifuge tube and blow dry at 40°C. Add.200μL of mobile phase A for reconstitution, centrifuge at 9700×g for 5min, take 100μL of the supernatant into a sample bottle, and take the supernatant for analysis. 6.1.1.1.2 Hair samples Shake and wash the hair sample twice with an appropriate amount of water and acetone in turn, dry it and cut it into approximately 1mm sections, weigh 20 mg of the hair sample into 2 mL In the grinding tube, add an appropriate amount of grinding beads, and then add 1 mL of the extraction solution containing 1ng/mL internal standard, freeze-grind with liquid nitrogen, centrifuge at 14000×g for 5 minutes, and take The supernatant is passed through a 0.22μm filter membrane, and the filtrate is directly supplied to the instrument for analysis. 6.1.1.2 Quality control samples 6.1.1.2.1 Body fluid samples Take two 100μL blank whole blood (or urine), one as a blank sample, and one with 10ng/mL of 31 new fentanyls 10μL of mixed standard working solution of psychoactive substances, prepared into 1ng/mL additive sample, and then according to 6.1.1.1.1 method, and case sample Parallel operation. 6.1.1.2.2 Hair samples Weigh two 20 mg blank hair samples, one as a blank sample, and one with 100 ng/mL 31 new fentanyl psychoactive substances 10μL of the qualitative mixed standard working solution was prepared to add 0.05ng/mg sample, and then operated in parallel with the case sample according to the method of 6.1.1.1.2. 6.1.2 Instrument testing 6.1.2.1 Instrument conditions 6.1.2.1.1 Liquid chromatography conditions 6.1.2.1.2 Mass spectrometry conditions Mass spectrometry conditions include. a) Ion source. electrospray ionization-positive ion mode (ESI); b) Detection method. multiple reaction monitoring (MRM); c) Ion source voltage (IS). 5500V; d) Collision gas (CAD), curtain gas (CUR), atomization gas (GS1), auxiliary gas (GS2) are all high-purity nitrogen, adjust each gas flow before use Mass to make the sensitivity of the mass spectrometer meet the detection requirements; e) The declustering voltage (DP) and collision energy (CE) should be optimized to the best sensitivity. Note. The mass spectrometry conditions can be adjusted according to the actual conditions of different instruments. 6.1.2.2 Sample injection Draw case samples, blank samples, and add sample extracts respectively, and analyze according to the conditions of 6.1.2.1. 6.1.2.3 Record Record the retention time and ion pair abundance ratio of the suspicious chromatographic peak of the target in each sample. 6.1.2.4 Basis for qualitative judgment The retention time, the characteristic fragment ion peak of the mass spectrum and the relative abundance ratio are used as the basis for qualitative judgment. If the chromatographic peaks of two pairs of qualitative ion pairs of the target substance appear in the case sample, the retention time and the color of the corresponding standard substance in the added sample Comparison of peak retention time, the relative error is within ±2.5%, and the qualitative ion pair abundance ratio is similar to the concentration of the ion pair abundance ratio of the added sample If the relative error does not exceed the range specified in Table 3, it can be determined that the target object exists in the case sample. 6.2 Quantitative analysis 6.2.1 Analysis method Use internal standard-working curve method or internal standard-single point calibration method for quantitative analysis. 6.2.2 Sample preparation Pipette (or weigh) two 100μL (or 20mg of hair) samples of the case sample blood/urine, according to 6.1.1.1.1 (or 6.1.1.1.2) Method operation. In addition, take several copies of the same matrix blank sample, add an appropriate amount of target substance, and obtain a series of mass concentration (mass fraction) or single-point mass concentration (Mass score) of the added sample is operated in parallel with the case sample. Refer to Appendix B for methodological validation data. The mass concentration (mass fraction) of the target substance in the case sample should be within the linear range of the working curve. Preparation of single point mass concentration (mass When adding samples to the sample, the mass concentration (mass fraction) of the target substance in the case samples should be within ± 50% of the mass concentration (mass fraction) Inside. 6.2.3 Instrument testing 6.2.3.1 Instrument conditions The instrument conditions should meet the requirements in 6.1.2.1. 6.2.3.2 Sample injection The case samples, serial mass concentration (mass fraction) addition samples, or single-point mass concentration (mass score) addition samples should be added separately, According to the conditions of 6.1.2.1 injection analysis. 6.2.4 Recording and calculation 6.2.4.1 Basic requirements The case sample, serial mass concentration (mass fraction) addition sample or single point mass concentration (mass score) addition sample should be recorded The peak area value of the target and internal standard, and then calculate the content. 6.2.4.2 Internal standard-working curve method In the series of added samples with mass concentration (mass fraction), the peak area ratio (Y) of the target and the internal standard quantitative ion pair should be taken as the vertical axis The mass concentration (mass fraction) (C) of the target and target substance is linear regression on the abscissa to obtain a linear equation. According to the peak area value of the target substance and the internal standard quantitative ion pair in each sample, calculate the mass concentration of the target substance in the case sample according to formula (1) (Quality score).7 Evaluation of analysis results7.1 Evaluation of qualitative analysis results 7.1.1 Evaluation of negative results Negative result evaluations include. a) If only the internal standard fentanyl-D5 and norfentanyl-D5 are detected in the case samples, and 31 target components are not detected, add the sample 31 new fentanyl-type psychoactive substances were detected in the test, the negative result is reliable; b) If the internal standard fentanyl-D5 and norfentanyl-D5 are not detected in the case sample, or 31 fentanyls are not detected in the added sample For new psychoactive substances, negative results are unreliable and should be retested according to 6.1. 7.1.2 Evaluation of positive results Evaluation of positive results includes. a) If one or more of 31 new fentanyl-type psychoactive substances are detected in the case sample and the blank sample has no interference, The positive result is reliable; b) If the blank sample is also positive, the positive result is unreliable and should be retested according to 6.1. 7.2 Evaluation of quantitative analysis results When the relative difference between the samples of the two cases does not exceed 20% (the corruption inspection material does not exceed 30%), the result is the average of the sample content of the two cases Value calculation, otherwise it should be re-measured. AAAppendix A(Informative appendix) Extracted ion chromatograms of 31 new psychoactive fentanyl substances and their metabolites The extracted ion chromatograms of 31 new fentanyl psychoactive substances and their metabolites are shown in Figure A.1. Note. Quantification limit concentration. body fluid 0.5ng/mL; hair 0.01ng/mg. Figure A.1 Extracted ion chromatograms of 31 new fentanyl-type psychoactive substances and their metabolites BBAppendix B(Informative appendix) Methodological validation data B.1 Working curve of body fluid sample The linear equation and linear range of body fluid samples are shown in Table B.1. ......Tips & Frequently Asked Questions:Question 1: How long will the true-PDF of SFT0066-2020_English be delivered?Answer: Upon your order, we will start to translate SFT0066-2020_English as soon as possible, and keep you informed of the progress. The lead time is typically 3 ~ 5 working days. The lengthier the document the longer the lead time.Question 2: Can I share the purchased PDF of SFT0066-2020_English with my colleagues?Answer: Yes. The purchased PDF of SFT0066-2020_English will be deemed to be sold to your employer/organization who actually pays for it, including your colleagues and your employer's intranet.Question 3: Does the price include tax/VAT?Answer: Yes. Our tax invoice, downloaded/delivered in 9 seconds, includes all tax/VAT and complies with 100+ countries' tax regulations (tax exempted in 100+ countries) -- See Avoidance of Double Taxation Agreements (DTAs): List of DTAs signed between Singapore and 100+ countriesQuestion 4: Do you accept my currency other than USD?Answer: Yes. If you need your currency to be printed on the invoice, please write an email to Sales@ChineseStandard.net. In 2 working-hours, we will create a special link for you to pay in any currencies. Otherwise, follow the normal steps: Add to Cart -- Checkout -- Select your currency to pay. |
