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GB 22175-2008: [GB/T 22175-2008] Diniconazole technical
Status: Valid
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[GB/T 22175-2008] Diniconazole technical
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GB 22175-2008
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Basic data | Standard ID | GB 22175-2008 (GB22175-2008) | | Description (Translated English) | [GB/T 22175-2008] Diniconazole technical | | Sector / Industry | National Standard | | Classification of Chinese Standard | G25 | | Classification of International Standard | 65.100.30 | | Word Count Estimation | 8,86 | | Date of Issue | 2008-07-11 | | Date of Implementation | 2009-01-01 | | Quoted Standard | GB/T 1250 | | 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 original drug diniconazole requirements, test methods and marking, labeling, packaging, storage and transportation. This standard applies to diniconazole its production process impurities consisting diniconazole original drug. | GB 22175-2008: [GB/T 22175-2008] Diniconazole 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.
Diniconazole technical
ICS 65.100.30
G25
National Standards of People's Republic of China
Diniconazole 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
Foreword
This standard Chapters 3 and 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. the Ministry of Agriculture.
Participated in the drafting of this standard. Jiang Su Jiannong Pesticide Chemical Co., Ltd., Jiangsu sword licensing pesticides Chemical Co., Ltd., Jiangsu Yancheng Limin
Chemical Co., Ltd.
The main drafters of this standard. One of Wei, Li Youshun, Wu Jinlong, paragraph Lifang, Zhou Jianhua, Xu Xiangsheng, Weihong Sheng.
The standard commission Secretariat of National Pesticide Standardisation Technical Committee responsible for the interpretation.
Diniconazole original drug
Other active ingredients of the product name Diniconazole, structural formula and basic physicochemical parameters are as follows.
ISO common name. diniconazole
CIPAC digital code. 690
Chemical Name. (E) - (RS) -1- (2,4- dichlorophenyl) -2- (1H-1,2,4- triazol-1-yl) -4,4-dimethyl pent-1-en-3-ol
Structure.
Empirical formula. C15H17Cl2N3O
Molecular Weight. 326.2 (according to 2005 international relative atomic mass)
Biological activity. bactericidal
Melting point. 134 ℃ ~ 156 ℃
Relative density. 1.32g/cm3 (20 ℃)
Vapor Pressure. 2.93mPa (20 ℃), 4.9mPa (25 ℃)
Solubility. Water 4mg/L (20 ℃), acetone 95g/kg (25 ℃), methanol 95g/kg (25 ℃), xylene 14g/kg (25 ℃),
Hexane 0.7g/kg (25 ℃)
Stability. light, heat, humidity and stability.
1 Scope
This standard specifies the diniconazole original drug requirements, test methods and marking, labeling, packaging and storage.
This standard applies to the impurities generated by the production process and diniconazole Diniconazole original drug thereof.
2 Normative references
The 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.
Representation GB/T 1250 limit values and the method of determining
GB/T 1600 Determination of Water Pesticides
Determination of GB/T 1601 Pesticides pH value
GB/T 1604 Goods pesticide regulations for acceptance
GB/T 1605 sampling commercial pesticides
GB 3796 pesticide packaging General
GB/T 19138 Determination of acetone insoluble pesticide
3 Requirements
3.1 Appearance. white to off-white powder, free from visible foreign matter.
3.2 diniconazole original drug should be consistent with the requirements in Table 1.
Table 1 diniconazole original drug control project indicators
Item Index
Diniconazole mass fraction /% ≥ 95.0
pH range of 5.0 to 8.0
Moisture /% ≤ 0.5
Fraction a /% by mass of acetone insolubles is ≤ 0.5
In a normal production conditions, the mass fraction of acetone insolubles test every three months, at least once.
Test Method 4
4.1 Sampling
Carried out according to GB/T 1605 "Product of the original drug sampling" method. Determined by sampling a random number table method packages, the final sample size should be a lot of
At 100g.
4.2 Identification Test
HPLC --- The identification test with diniconazole determination simultaneously. Under the same chromatographic operating conditions, the sample
One solution peak retention time compared with standard sample solution diniconazole chromatographic retention time, the relative difference should be less than 1.5%.
Infrared spectroscopy --- sample and standard samples in the infrared range 4000cm-1 ~ 400cm-1 absorption spectrum should be no significant differences (see
FIG. 1)
Figure 1 diniconazole standard infrared spectrum
4.3 Determination of the mass fraction of diniconazole
4.3.1 Method summary
Sample dissolved in mobile phase, methanol + water as the mobile phase, use as filler to C18 stainless steel column and UV detector (250nm),
Other than the standard method of sample diniconazole reverse phase HPLC separation and determination.
4.3.2 Reagents and solutions
Methanol. HPLC grade;
Water. The new secondary steam distilled water;
Diniconazole standards. a known mass fraction ≥99.0%.
4.3.3 Instruments
High performance liquid chromatography. a variable wavelength UV detector;
Chromatographic data processor or chromatography workstation;
Column. 250mm × 4.6mm (. I.d) stainless steel column, built ZORBAXSB-C185μm filler (or other equivalent effect
Column);
Filter. filter pore size of about 0.45μm;
Micro injector. 50μL;
Ultrasonic cleaner.
4.3.4 HPLC operating conditions
Mobile phase. (methanol. water) = 85.15, by membrane filtration, and degassing;
The mobile phase flow rate. 1.0mL/min;
Column temperature. room temperature (temperature change should not exceed 2 ℃);
Detection wavelength. 250nm;
Injection volume. 5μL;
Retention time. Diniconazole about 5.6min, diniconazole isomers about 4.5min.
It said operating parameters are typical, according to the characteristics of different instruments and columns for a given operating parameters adjusted as appropriate, in order to obtain the most
Good effect. Typical diniconazole original drug HPLC is shown in Figure 2.
1 --- Diniconazole isomer;
2 --- diniconazole.
Figure 2 diniconazole original drug HPLC chromatogram
4.3.5 measuring step
4.3.5.1 Sample solution preparation
Weigh diniconazole standards 0.05g (accurate to 0.0002g), placed in 100mL volumetric flask, dissolved in mobile phase and dilute to the mark,
Shake well.
4.3.5.2 Sample solution preparation
Weigh the sample containing diniconazole 0.05g of (accurate to 0.0002g), placed in 100mL volumetric flask, dissolved in mobile phase and dilute to
Mark and shake.
4.3.5.3 Determination
Under these operating conditions, after the instrument is stable, continuous injection of several doses of the standard solution until the two adjacent needles diniconazole peak area relative change
After less than 1.5%, according to the solution, sample solution, sample solution, standard order of standard solution was measured.
4.3.6 Calculation
Before and after the two-pin solution and the sample solution in the sample measured two doses of the standard solution diniconazole peak areas are averaged. Sample ene
Yl alcohol content of 1 (%) according to equation (1).
1 = A2
(1)
Where.
Two doses of the standard solution A1 --- alcohol before and after diniconazole mean peak area;
Sample solution before and after the two-pin A2 --- diniconazole mean ol peak area;
--- Standard Diniconazole mass fraction, expressed as a percentage.
4.3.7 allowable difference
The difference between two parallel determination results shall not be greater than 1.2%, the arithmetic mean value as a measurement result.
4.4 Determination of Moisture
According to GB/T 1600 in the "Karl Fischer method".
According to GB/T 1601 carried out.
4.6 Determination of acetone insoluble mass fraction
According to GB/T 19138 performed.
4.7 product testing and acceptance
Shall comply with GB/T 1604's. Treatment of extreme values using GB/T 1250 rounding value comparison method.
5 marking, labeling, packaging, storage and transportation
Flag 5.1 diniconazole original drug, labeling and packaging should comply with the relevant provisions of GB 3796.
5.2 diniconazole original drug application of clean, dry, or cardboard drums lined with plastic bag, net weight 25kg. Can also
User requirements or orders protocol, using other forms of packaging, subject to the relevant provisions of GB 3796.
5.3 The package should be stored in 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. diniconazole low toxicity fungicides, skin, eye irritation symptoms. The FDA should wear protective gloves. After contact with skin, should stand
That wash with soap and water; if splashed into the eyes, rinse with plenty of water; if orally ingested to induce vomiting and sent to hospital symptomatic treatment.
5.6 Acceptance Period. diniconazole original drug acceptance period of 1 month. From the date of delivery, within one month, the finished product quality inspection, its means
Standard shall meet the standards.
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