Analytical method of Chlorfenapyr in Suspension Concentrate

1. Outline of method
A HPLC method was developed for determination of Chlorfenapyr content in
Suspension concentrate by using ODS – C18 stainless steel column, a variable
wavelength UV detector, Acetonitrile + Water + Glacial acetic acid = (75 + 25 + 0.1)
as the mobile phase, and an external standard.
2. Reagent and Solution
Acetonitrile: Chromatographic reagent;
Glacial acetic acid: Chromatographic reagent;
Water: Double-distilled water or ultrapure water;
Chlorfenapyr Standard with known purity.
3. Apparatus
High Performance Liquid Chromatography (HPLC) with variable wave-length UV
detector;
Chromatographic data processor;
Chromatographic column: 150mm x 4.6mm (i.d.), ODS-C18 stainless steel column;
Filter: Filter membrane porosity 0.45 μm;
Micro-injector: 5 μL
Ultrasonic cleaner
4. Operating conditions of HPLC (typical)
Mobile phase: φ(acetonitrile + water + glacial acetic acid = (75 +25 +0.1)
Flow rate: 1.0 mL/min
Column temperature: Ambient temperature
Injection volume: 5μL
Detector wavelength: 260nm
Retention time: Chlorfenapyr about 5.5 min
5. Testing approach
(a) Standard solution preparation
Weigh accurately 0.05g (to the nearest 0.0001g) of standard Chlorfenapyr into a
100ml volumetric flask, dissolve with 80ml acetonitrile and dilute to the mark with
acetonitrile, shake well.
(b) Sample solution preparation
Weigh enough Chlorfenapyr sample to contain 0.05g (to the nearest 0.0001g) of
Chlorfenapyr into a 100ml volumetric flask, add 5ml water, dissolve with 80ml
acetonitrile and dilute to the mark with acetonitrile, shake well, filter with filter
membrane porosity 0.45 μm, wait for test.
(c) Determination
Under the above operating conditions, continuously inject a number of needles of
standard sample after the instrument is stable, the relative change of peak area of two
adjacent needles of Chlorfenapyr is less than 1.5%, determinate in the following
sequence: standard sample, sample, sample, standard sample.
6. Calculation
Calculate the average peak area of two needles of sample solutions, two needles of
standard solution front and back of sample solutions, respectively. Calculate the
content X1 of Chlorfenapyr using the following formula:

A1  m s  p
X1=
A2  m1

Where:
A1 = the peak area’s average value of Chlorfenapyr standard sample solution;
A2 = the peak area’s average value of Chlorfenapyr sample solution;
m1 = mass of Chlorfenapyr standard sample (g);
m2 = mass of Chlorfenapyr sample (g);
p = Purity of Chlorfenapyr standard sample (%).