GB 24752-2009Methomyl technical (English PDF)

3.1 Appearance

White to off-white crystalline powder.

3.2 Technical Specifications

Methomyl original drug should also meet the requirements of Table 1.

Table 1 Methomyl original drug control project indicators

Item Index

Methomyl content /% >= 98.0

Acetone insolubles a /% <= 0.2

Moisture /% <= 0.3

The pH range of 4.0 to 8.0

When a normal production, the acetone insoluble matter was detected at least once every three months.

Test Method 4

4.1 Sampling

Carried out in GB/T 1605-2001 of "original drug product sampling" approach. Determined by sampling a random number table method packages, the amount of the final sample

Not less than 100g.

4.2 Identification Test

The present liquid chromatography --- identification test can be carried out simultaneously with the determination of the mass fraction of methomyl. Chromatography under the same operating conditions, the test

A solution sample peak retention time of the standard solution Methomyl retention time, the relative difference should be less than 1.5%.

Infrared spectroscopy --- Methomyl sample and standard IR in the range of 4000cm-1 ~ 400cm-1 absorption spectrum should be no significant difference

different. Methomyl standard infrared spectra of Figure 1.

Figure 1 methomyl standard infrared spectrum

4.3 Determination of the mass fraction of methomyl

4.3.1 Method summary

Sample was dissolved in methanol, methanol + water as the mobile phase, used as a filler SpherisorbC8 stainless steel column and UV detector

(235nm), the sample methomyl reverse phase high performance liquid chromatography and determination.

4.3.2 Reagents and solutions

Methanol. HPLC grade;

Water. The new secondary steam distilled water;

Methomyl Standard. Known methomyl content, >=99.0%.

4.3.3 Instruments

HPLC. a variable wavelength UV detector;

Chromatographic data processor or chromatography workstation;

Column.200mm × 4.6mm (. I.d) stainless steel column, SpherisorbC8,10µm filler contents (or with equivalent effect

C8, C18 bonded phase);

Filter. membrane pore size of about 0.45 m;

Microsyringe. 50µL;

Quantitative sampling tube. 5µL;

Ultrasonic cleaning.

4.3.4 HPLC operating conditions

Mobile phase. [Psi] (methanol. water) = 40.60, by membrane filtration, and degassing;

Flow rate. 1.0mL/min;

Column temperature. room temperature (temperature change should be less than 2 deg.] C);

Detection wavelength. 235nm;

Injection Volume. 5µL;

Retention time. Methomyl about 4.1min.

Are typical operating parameters of the above, according to the characteristics of different instruments, for a given operating parameters appropriately adjusted to obtain the best result.

Typical methomyl original drug by HPLC is shown in Figure 2.

4.3.5 Determination Step

4.3.5.1 Preparation of standard solution

Weigh 0.10 g methomyl standard (accurate to 0.0002g), a 50mL volumetric flask, diluted with methanol to the mark. accurate

The solution was pipetted 10mL, 50mL volumetric flask, diluted with methanol to the mark.

4.3.5.2 Preparation of sample solution

Methomyl containing weighed about 0.10g sample of the original drug (accurate to 0.0002g), a 50mL volumetric flask, dilute to the mark with methanol

Degree, shake. The solution was accurately pipetted 10mL, 50mL volumetric flask, diluted with methanol to the mark.

4.3.5.3 Determination

Under the above operating conditions, after the instrument is stable, the number of consecutive doses of the standard solution is injected until the two needles methomyl relative change in peak area adjacent

After less than 1.5%, measured according to the standard solution, sample solution, the sample solution, the order of standard solution.

4.3.6 computing

The two needle and the sample solution was measured before and after the two doses of the standard sample solution Methomyl peak area are averaged. Sample Methomyl

A mass fraction (%), according to equation (1).

4.3.7 allows poor

Results difference methomyl replicates should be less than twice the mass fraction of 1.2%, and the arithmetic mean value as a measurement result.

4.4 Determination of acetone insolubles

According to GB/T 19138 carried out.

4.5 Determination of Moisture

According to GB/T 1600 in the "Karl Fischer method".

Carried out in GB/T 1601.

4.7 product testing and acceptance

Shall comply with the provisions of GB/T 1604's. Limit values rounding processing using the value comparison method.

5.3 methomyl original drug package airiness, dry place.

5.4 storage and transportation to prevent moisture and sunlight, no food, seed, feed mix, avoid contact with skin, eyes, nose and mouth to prevent inhalation.

5.5 Security. instructions for use in or on a packaging container, in addition to the respective signs of toxicity, there should be about the toxicity as follows.

Methomyl is highly toxic carbamate pesticides, toxic inhalation, eating can be deadly. The FDA should avoid direct contact with skin and eyes

Touch, Do not breathe dust and spray. All operations should be carried out in the ventilation, and skin and eye protection to take appropriate measures in case of contact,

Washed with water 15min, then washed with soap and skin, and receive medical treatment. Atropine is a specific antidote.

5.6 Acceptance period. Methomyl original drug acceptance period of one month. From the date of delivery, product quality inspection completed within a month, the indicators

Shall meet the standards.

END: Draft Version (GB 24752-2009)