50g/L Lambdacyhalothrin EC analytical method

1.1.1 Determination of Lambdacyhalothrin content

Summary of method

The sample was dissolved with a mixture of petroleum ether + trichloromethane

reagent.

The sample was dissolved with a mixture of petroleum ether + trichloromethane

reagent, and the Lambdacyhalothrin in the sample was separated and sidetracked by

normal-phase high-performance liquid chromatography (NP-HPLC). sidetracked by

normal-phase high-performance liquid chromatography (NP-HPLC) using a stainless

steel column packed with silica gel and an ultraviolet detector with n-phase high-

performance liquid chromatography. ultraviolet detector with n-hexane +

tetrahydrofuran solvent mixture as the mobile phase.

1.1.2 Reagents and solutions

Petroleum ether: analytically pure

Tetrahydrofuran: analytically pure

n-hexane: analytically pure

Solvent: petroleum ether + trichloromethane = 90 + 10 (v/v)

Lambdacyhalothrin specimen: known mass fraction ≥96%.

1.1.3 Instruments, equipment

High performance liquid chromatograph: with variable wavelength ultraviolet

detector.

Chromatographic column:250mm×4.6mm(id) stainless steel column with Nova-

Pak SiO2 5µm filler.

Chromatographic data processor.

Quantitative injection tube: 20µL.

Ultrasonic cleaner.

1.1.4 High performance liquid chromatography operating conditions

Mobile phase: n-hexane + tetrahydrofuran = 500 + 5 (v/v).

Flow rate: 3.0mL/min.

Column temperature: room temperature

Detection wavelength: 230nm

Injecting volume: 20µL.

The above operating parameters are typical, and the given operating parameters

can be adjusted appropriately according to the characteristics of different instruments

to obtain the best results.

1.1.5 Measurement steps

1.1.5.1 Preparation of the standard solution

Weigh 0.03g of Lambdacyhalothrin sample (in percent, accurate to 0.0001g), put

it into a 50mL volumetric flask, dilute with solvent and dissolve it with ultrasonic

shaking.

1.1.5.2 Preparation of sample solution

 Weigh about 0.03g of Lambdacyhalothrin sample (100 percent, accurate to

0.0001g), placed in a 50mL volumetric flask, with solvent dilution and capacity of

ultrasonic shaking to fully dissolve the test.

Under the above operating conditions, after the baseline of the instrument is

stabilized, inject several needles of standard sample solution continuously until the

relative response value change of two adjacent needles is less than 1.5%, and then

feed the sample in the following order: standard sample solution, test sample solution,

test sample solution, standard sample solution.

1.1.6 Calculation

The peak areas of Lambdacyhalothrin in the measured two-needle specimen

solution and in the two-needle standard solution before and after the specimen were

averaged separately.

The mass fraction of Lambdacyhalothrin in the specimen (X1) was calculated

according to equation (1).

A2×m1×P
X1 = …………………………………………………
A1×m2

Eq:

A1 - mean value of Lambdacyhalothrin peak area in the standard sample

solution;

A2 - average value of Lambdacyhalothrin peak area in the specimen solution;

m1 - mass of the Lambdacyhalothrin standard sample in grams (g);

m2 - mass of the specimen in grams (g);

P- Mass fraction of Lambdacyhalothrin in the standard sample, %.