SFT0065-2020 English PDFUS$439.00 · In stock
Delivery: <= 4 days. True-PDF full-copy in English will be manually translated and delivered via email. SFT0065-2020: (Liquid Chromatography-Tandem Mass Spectrometry Test Method for 16 Kinds of New Tryptamines and Their Metabolites in Hair, such as Dimethyltryptamine) Status: Valid
Basic dataStandard ID: SF/T 0065-2020 (SF/T0065-2020)Description (Translated English): (Liquid Chromatography-Tandem Mass Spectrometry Test Method for 16 Kinds of New Tryptamines and Their Metabolites in Hair, such as Dimethyltryptamine) Sector / Industry: Chinese Industry Standard (Recommended) Classification of Chinese Standard: C06 Word Count Estimation: 19,183 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 SFT0065-2020: (Liquid Chromatography-Tandem Mass Spectrometry Test Method for 16 Kinds of New Tryptamines and Their Metabolites in Hair, such as Dimethyltryptamine)---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 16 tryptamine hallucinogens and their metabolites in hair samples by liquid chromatography- tandem mass spectrometry ICS 07.140 C 06 SF People's Republic of China judicial administration industry standards 16 kinds of tryptamines in hair such as dimethyl tryptamine Detection of sexual substances and their metabolites by liquid chromatography-tandem mass spectrometry Test 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...2 7 Evaluation of analysis results...6 Appendix A (informative appendix) The extracted ion current diagrams of 16 new tryptamine psychoactive substances and their metabolites...8 Appendix B (informative appendix) Methodological validation data...13ForewordThis 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. A solution of 16 new tryptamine psychoactive substances and their metabolites in hair, including dimethyltryptamine Gas chromatography-tandem mass spectrometry method1 ScopeThis standard specifies the liquid chromatography-tandem mass spectrometry of 16 new tryptamine psychoactive substances and their metabolites such as dimethyltryptamine in hair (LC-MS/MS) Reagents, instruments and materials, operation methods and analysis results evaluation requirements for inspection. This standard applies to the qualitative and quantitative analysis of 16 new tryptamine psychoactive substances and their metabolites in hair, such as dimethyltryptamine. Other The qualitative and quantitative analysis of 16 new tryptamine psychoactive substances and their metabolites, including dimethyltryptamine, 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 hair samples are extracted by organic solvents, they are detected by liquid chromatography-tandem mass spectrometry (LC-MS/MS). The white sample and the added sample were compared, and the retention time and relative abundance ratio of the two parent ion/daughter ion pairs were used for qualitative analysis; Based on the sub-pair peak area, 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. rotation speed 14000×g; d) Ultrasonic cleaner; e) 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 Wash the hair sample twice with an appropriate amount of water and acetone shaking in turn, dry it and cut it into about 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 Weigh two 20 mg blank hair samples, one as a blank sample, and one with 10 μL of 100 ng/mL 16 kinds of tryptamines. The mixed standard working solution of sexual substances is prepared to add 0.05ng/mg sample, and then follow the method 6.1.1.1 to operate in parallel with the case sample. 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. Under the chromatographic and mass spectrometric conditions of 6.1.2.1.1 and 6.1.2.1.2, 16 new tryptamine psychoactive substances and their metabolites and internal standards The qualitative ion pairs, quantitative ion pairs and retention times of the qualitative ion pairs are shown in Table 2.The MRM chromatograms of the 16 target compounds are shown in Appendix A. 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 Quantitative analysis was performed using internal standard-working curve method or internal standard-single point calibration method. 6.2.2 Sample preparation Weigh two copies of 20 mg hair of the case sample, and the remaining sample pretreatment is the same as 6.1.1.1. In addition, take several copies of blank hairs of the same matrix, add appropriate amount of target substance, and prepare additional samples with serial mass score or single-point mass score. Operate in parallel with case samples. Refer to Appendix B for methodological validation data. The mass score of the target in the case sample should be within the linear range of the working curve. When preparing an additive sample with a single point mass score, the case The mass fraction of the target substance in the sample should be within ±50% of the mass fraction. 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, the added samples of the series of mass scores, or the single-point mass scores of the added samples should be added separately, and the samples should be injected according to the conditions of 6.1.2.1 Analysis. 6.2.4 Recording and calculation 6.2.4.1 Basic requirements The peak area value of the target substance and internal standard in the case sample, the added sample of the series mass score or the single-point mass score added sample should be recorded. Then calculate the content. 6.2.4.2 Internal standard-working curve method In the added samples with a series of mass fractions, the peak area ratio (Y) of the target substance and the quantitative ion pair of the internal standard should be taken as the ordinate and the target substance The quantity score (C) 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, the mass fraction of the target substance in the case sample is calculated according to formula (1). 6.2.4.3 Internal standard-single point calibration method According to the peak area value of the target substance and the internal standard quantitative ion pair in the case sample and the added sample, the target in the case sample should be calculated according to formula (2). The mass score of the target.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 standards siloxibin-d4 and siloxin-d10 are detected in the sample of the case, and 16 target components are not detected, add them to the sample If 16 kinds of tryptamine new psychoactive substances are detected, the negative result is reliable; b) If the internal standards siloxibin-d4 and siloxin-d10 are not detected in the sample of the case, or 16 new tryptamines are not detected in the added sample If the negative result is unreliable, it should be tested again according to 6.1. 7.1.2 Evaluation of positive results Evaluation of positive results includes. a) If one or more of the 16 new tryptamine psychoactive substances is detected in the case sample and the blank sample has no interference, then The positive result is judged to be 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 result shall be calculated as the average of the contents of the samples of the two cases, otherwise it shall be determined again. AAAppendix A(Informative appendix) Extraction ion chromatograms of 16 new tryptamine psychoactive substances and their metabolites The extracted ion current diagrams of 16 new tryptamine psychoactive substances and their metabolites are shown in Figure A.1. Note. Limit of quantification. 0.05ng/mg for hairAppendix B(Informative appendix) Methodological validation data B.1 Working curve of detection methods for 16 new tryptamine psychoactive substances and their metabolites in hair The linear equation and linear range are shown in Table B.1. B.2 Method accuracy, precision, recovery rate and matrix effect The precision, accuracy, recovery and matrix effect of the method are shown in Table B.2. ......Tips & Frequently Asked Questions:Question 1: How long will the true-PDF of SFT0065-2020_English be delivered?Answer: Upon your order, we will start to translate SFT0065-2020_English as soon as possible, and keep you informed of the progress. The lead time is typically 2 ~ 4 working days. 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