GB 22172-2008 English PDFUS$239.00 · In stock
Delivery: <= 3 days. True-PDF full-copy in English will be manually translated and delivered via email. GB 22172-2008: [GB/T 22172-2008] Paclobutrazol technical Status: Valid
Basic dataStandard ID: GB 22172-2008 (GB22172-2008)Description (Translated English): [GB/T 22172-2008] Paclobutrazol technical Sector / Industry: National Standard Classification of Chinese Standard: G25 Classification of International Standard: 65.100.20 Word Count Estimation: 9,995 Date of Issue: 2008-07-11 Date of Implementation: 2009-01-01 Quoted Standard: GB/T 1601; GB/T 1604; GB/T 1605-2001; GB 3796; GB/T 19138 Regulation (derived from): Announcement of Newly Approved National Standards No. 12 of 2008 (No. 125 overall) Issuing agency(ies): General Administration of Quality Supervision, Inspection and Quarantine of the People's Republic of China, Standardization Administration of the People's Republic of China Summary: This Chinese standard specifies the requirements for MET original drug, test methods and marking, labeling, packaging, storage and transportation. This standard applies to the MET and impurities generated in the production of MET original drug. GB 22172-2008: [GB/T 22172-2008] Paclobutrazol technical---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.Paclobutrazol technical ICS 65.100.20 G25 National Standards of People's Republic of China MET original drug Posted 2008-07-11 2009-01-01 implementation Administration of Quality Supervision, Inspection and Quarantine of People's Republic of China Standardization Administration of China released ForewordThe standard Chapter 3, Chapter 5 are mandatory, the rest are recommended. The standard proposed by China Petroleum and Chemical Industry Association. This standard by the National Standardization Technical Committee on Pesticides (CSBTS/T C133) centralized. This standard is drafted by. Shenyang Chemical Research Institute. Participated in the drafting of this standard. Sichuan Chemical Industry Research and Design Institute, Jiang Su Jiannong pesticides Chemical Co., Ltd., Jiang Su Qizhou green Engineering Co., Ltd., Jiangsu sword licensing pesticides Chemical Co., Ltd. The main drafters of this standard. to Xu Wei, Zhang Xuebing, Xing Hong, Duan Xiu Hong, Xu Xiangsheng, Chenru Juan, Zhou Jianhua, Hu Chunhong. The standard commission Secretariat of National Pesticide Standardisation Technical Committee responsible for the interpretation. MET original drug Other name, structural formula and basic physicochemical parameters of the active ingredient paclobutrazol product as follows. ISO common name. paclobutrazol CAS Registry Number. [76738-62-0] Chemical name. (2RS, 3RS) -1- (4- chlorophenyl) -4,4-dimethyl -2- (1H-1,2,4- triazol-1-yl) pentan-3-ol Structure. Empirical formula. C15H20ClN3O Molecular Weight. 293.8 (according to 2005 international relative atomic mass) Biological activity. Plant Growth Regulator Melting point. 165 ℃ ~ 166 ℃ Vapor Pressure. 1μPa (20 ℃) The relative density (25 ℃). 1.22 Solubility (20 ℃, g/L). water, 2.6 × 10-2, 110 acetone, cyclohexanone, 180, 100 methylene chloride, hexane 10, xylene 60, 150 methanol, propylene glycol 50 Stability. 20 ℃ storage stable for more than 2 years; 50 ℃ stored for 6 months or more stable; in pH4 ~ pH9 water stable; at pH7 Article 10d do not degrade under UV irradiation member1 ScopeThis standard specifies the requirements for MET original drug, test methods and marking, labeling, packaging, storage and transportation. This standard applies to the impurities generated in the production of MET and MET composed the original drug.2 Normative referencesThe following documents contain provisions which, through reference in this standard and become the standard terms. For dated references, subsequent Amendments (not including errata content) or revisions do not apply to this standard, however, encourage the parties to the agreement are based on research Whether the latest versions of these documents. For undated reference documents, the latest versions apply to this standard. Determination of GB/T 1601 Pesticides pH value GB/T 1604 Goods pesticide regulations for acceptance GB/T 1605-2001 Sampling Method commercial pesticides GB 3796 pesticide packaging General GB/T 19138 Determination of acetone insoluble pesticide3 Requirements3.1 Composition and Appearance. This product should be related to the production of MET and impurities, should be white to tan solid, no visible foreign matter and Filling modifier. 3.2 MET original drug should be consistent with the requirements in Table 1. Table 1 MET original drug quality control program indicators Item Index MET mass fraction /% ≥ 95.0 Loss on drying /% ≤ 0.5 pH range 4.0 to 9.0 Acetone insolubles a /% ≤ 0.5 When a normal production, insoluble in acetone was tested once every three months at least. Test Method 4 4.1 Sampling According to GB/T 1605-2001 "on the original drug product sampling" approach. Determining sample package using a random number table method; the final sample size Not less than 250g. 4.2 Identification Test IR spectra of infrared spectroscopy --- sample with MET standard infrared spectra (see Figure 1), there should be no significant difference. Liquid chromatography --- The identification test can be carried out simultaneously with the determination of MET Quality Score. Under the same chromatographic operating conditions, the test The retention time of the sample solution and the standard solution to a peak in the MET peak retention time, the relative difference should be less than 1.5%. Gas Chromatography --- The identification test can be carried out simultaneously with the determination of MET Quality Score. Under the same chromatographic operating conditions, the test The retention time of the sample solution and the standard solution to a peak in the MET peak retention time, the relative difference should be less than 1.5%. Figure 1 standard infrared spectra of MET Determination of the mass fraction of 4.3 MET 4.3.1 Liquid Chromatography (Arbitration Act) 4.3.1.1 Method summary Sample was dissolved in methanol, methanol - acetonitrile - water as mobile phase, the choice of Nova-pakC18,5μm stuffing column and UV variable Wavelength detector to sample the MET liquid chromatography separation and determination. 4.3.1.2 Reagents and solutions Methanol. HPLC grade; Acetonitrile. chromatographic pure; Water. The new secondary steam distilled water; MET standard. a known mass fraction ≥99.0%. 4.3.1.3 Instruments LC. a variable wavelength UV detector and quantitative injection valve; Chromatographic data processor or chromatography workstation; Column. 3.9mm (id) × 150mm stainless steel columns, built-Nova-pakC18,5μm filler (or a column with the same efficiency He reversed-phase column); Ultrasonic bath; Micro Injector. not less than 50μL. 4.3.1.4 LC operating conditions Mobile phase. ψ (CH3OH.CH3CN.H2O) = 35.20.45; The mobile phase flow rate. 1.0mL/min; Column temperature. room temperature (temperature change should not exceed 2 ℃); Detection wavelength. 230nm; Injection volume. 10μL; Retention time (min). 4-H 3.8 MET, MET Ⅱ body 6.3, 7.7 MET, chlorine trazodone 9.6. HPLC operating conditions described above, the Department of typical operating parameters. According to the characteristics of different instruments, given operating parameters adjusted as appropriate, In order to obtain the best results. Typical liquid chromatogram MET original drug is shown in Figure 2. 1 --- 4-H MET; 2 --- MET Ⅱ body; 3 --- MET; 4 --- chlorine trazodone. Figure 2 MET liquid chromatogram of the original drug 4.3.1.5 Measurement procedure 4.3.1.5.1 preparation of standard solution Weigh MET standard 0.10g (accurate to 0.0002g), a 50mL volumetric flask, add 40mL of methanol, in an ultrasonic Bath sonication 5min. Remove cooled to room temperature, add methanol to volume, shake; pipette imbibe 5mL, set another 50mL volumetric flask, add methanol to volume, shake. 4.3.1.5.2 preparation of the sample solution Weigh the sample 0.10g (accurate to 0.0002g), a 50mL volumetric flask, add 40mL of methanol, in an ultrasonic bath Sonication 5min. Remove cooled to room temperature, add methanol to volume, shake; pipette imbibe 5mL, set another 50mL Volumetric flask, add methanol to volume, shake. 4.3.1.5.3 Determination Under the above chromatographic operating conditions, after the instrument is stable, continuous injection of several doses of the standard solution until the two adjacent needles MET relative peak area After the change is less than 1.0%, according to the order of the standard solution, sample solution, sample solution, standard solution injection analysis. 4.3.1.6 Calculation The two needle sample solution measured before and after the peak area of the sample and two doses of the standard solution MET are averaged. Sample pleiotropic Azole mass fraction of 1 (%) according to equation (1). (1) Where. A1 --- the average peak area of standard solution MET; The average peak area A2 --- MET in the sample solution; --- Paclobutrazol standard mass fraction, expressed as a percentage. 4.3.1.7 allowable difference The difference between two parallel determination results shall not be greater than 1.2%, the arithmetic mean value as a measurement result. 4.3.2 Gas Chromatography 4.3.2.1 Method summary Sample was dissolved in chloroform to triphenylmethane as the internal standard, using a HP-5 (5% + 95% diphenyl dimethyl polysiloxane) painted walls Quartz capillary column and flame ionization detector to sample the MET gas chromatography separation and determination. 4.3.2.2 Reagents and solutions Chloroform; Triphenylmethane. Do not interfere with the analysis of impurities; Internal standard solution. Weigh 5.8g triphenylmethane, in 1000mL volumetric flask with chloroform dissolved and diluted to scale, shake; MET standard. a known mass fraction ≥99.0%. 4.3.2.3 Instruments Gas chromatograph. with a hydrogen flame ionization detector; Column. 30m × 0.32mm (i.d.) Quartz capillary column, wall coated HP-5 (5% diphenyl + 95% dimethyl polysiloxane), membrane Thick 0.25μm; Chromatographic data processor or chromatography workstation. 4.3.2.4 GC operating conditions Column compartment temperature (temperature programming). initial 200 ℃, holding 8min; then to 20 ℃/min temperature is increased up to 250 ℃, 7min maintained; Gasification chamber temperature. 280 ℃; Detector temperature. 280 ℃; Gas flow rate (mL/min). carrier gas (N2) 2.0, hydrogen gas 30, air 300, the compensation gas (N2) 25; Split ratio. 40.1; Injection volume (μL). 1.0; Retention time (min). internal standard 5.0, chlorine trazodone 5.6, 6.9 MET, MET MET Ⅱ body 7.2,4-H 14.0. GC operating conditions described above, the Department of typical operating parameters. According to the characteristics of different instruments, given operating parameters adjusted as appropriate, In order to obtain the best results. MET typical gas chromatogram of the original drug is shown in Figure 3. 1 --- internal standard (triphenylmethane); 2 --- chlorine trazodone; 3 --- MET; 4 --- MET Ⅱ body; 5 --- 4-H MET. Figure 3 MET gas chromatogram of the original drug 4.3.2.5 Measurement procedure 4.3.2.5.1 preparation of standard solution Weigh MET standard 0.10g (accurate to 0.0002g), was placed in a 15mL stoppered glass bottle with a pipette accurately added 10mL internal standard solution, dissolve, shake. 4.3.2.5.2 preparation of the sample solution Weigh a sample containing 0.10g MET (accurate to 0.0002g), was placed in a 15mL stoppered glass vial, with the same 4.3.2.5.1 A pipette accurate internal standard solution was added 10mL dissolved, shake. 4.3.2.5.3 Determination Under these operating conditions, the instrument until a stable baseline, the number of continuous injection doses of the standard solution, calculate the MET needle and the internal standard peak area Repeatability than when the relative changes in the MET standard peak area ratio of less than 1.2%, according to the standard solution, sample solution to be two adjacent needles, The sample solution, the order of the standard solution was measured. 4.3.2.6 Calculation The two needle sample solution and measured before and after the two doses of the standard sample solution MET and the internal standard peak area ratios were averaged. test MET sample mass fraction of 1 (%) according to equation (2). 1 = γ2 (2) Where. γ1 --- standard solution, MET and the internal standard peak area ratio of the average; γ2 --- sample solution, MET and the internal standard peak area ratio of the average; --- Paclobutrazol standard mass fraction, expressed as a percentage. 4.3.2.7 allowable difference Twice the difference between the results of the mass fraction of MET parallel determination, should not exceed 1.2%, and the arithmetic mean as a measurement result. 4.4 Determination of loss on drying 4.4.1 Instruments and Appliances Weighing bottle. diameter 50mm, height 20mm; Oven. 100 ℃ ± 2 ℃; Dryer. 4.4.2 Procedure The weighing bottle placed in 100 ℃ ± 2 ℃ oven baking 1h, and then into the dryer to cool to room temperature, weighed (accurate to 0.0001g). Repeat the above steps until constant weight weighing bottle. In weighing bottle was weighed into a 10g sample (paved weighed accurate to 0.0001g). Will be referred Flask back into the oven and bake uncovered 1h, the lid is removed and placed in a dryer 0.5h cooled weighed (accurate to 0.0001g). repeat The operation until the weighing bottle and the sample constant weight. 4.4.3 Calculation 2 samples of loss on drying (%) according to equation (3) Calculated. 100 (3) Where. According to GB/T 1601 carried out. 4.6 Determination of acetone insolubles According to GB/T 19138 performed. 4.7 product testing and acceptance Product inspection and acceptance shall comply with GB/T 1604's. Treatment of extreme values, using the rounding value comparison method. 5 marking, labeling, packaging, storage and transportation 5.1 MET sign the original drug, labeling, packaging shall comply with the provisions of GB 3796. MET original drug use clean plastic buckets lined with plastic or iron Pail, careful not to make direct contact with the metal. Net weight 50kg per barrel ships or 200kg. 5.2 is also available upon request or order agreement, the use of other forms of packaging, subject to the provisions of GB 3796. 5.3 MET original drug package should be stored in well-ventilated, dry coffers. 5.4 storage, prevent moisture and sunlight, no food, seed, feed mix, avoid contact with skin, eyes, mouth and nose to prevent inhalation. 5.5 Security. This product is a low-toxic pesticides, are swallowed and inhaled toxic. When using this product to wear goggles and rubber gloves and other necessary Protective clothing. Such as skin, eyes accidentally stained with the product, rinse immediately with plenty of water. Coverage were immediately sent to hospital for treatment. 5.6 of acceptance. Acceptance of MET original drug for a month. From the date of delivery, product quality inspection completed within a month, its Indicators should meet the standards. ...... |
