7.6.25
) into 50 mL volumetric flask, add H2O to
AOAC Official Method 984.06
Dalapon (Magnesium and/or Sodium Salt)
in Pesticide Formulations
Liquid Chromatographic Method
First Action 1984
Final Action 1987
A. Principle
Dalapon is separated from related compounds on reverse phase
LC col umn, using paired-ion eluant, and measured by UV
spectrophotometry.
B. Apparatus
(a) Liquid chromatograph.—With 214 nm UV detector, 20 mL
in jec tor and chart re corder. Com puting in te gra tor op tional.
Operating conditions: temperature, 20°–30°C; eluant flow rate,
160 mL/h; detector sensitivity, 0.25 AUFS.
(b) Liquid chromatographic columns.—50 ´ 4.6 (id) mm Co:Pell
ODS pellicular guard column (No. 6561-404, Whatman, Inc.); 100 ´
8 (id) mm C18, 10 mm radial compression main column with
RCM-100 column holder (Waters Associates, or equivalent [such as
Whatman Partisil 10 ODS-3]). Columns slowly degrade in use.
Replace when 30% loss of retention occurs and repack first 5 mm of
guard column. Radial compression column recommended gives lower
back-pressure and longer column life than standard 316 stainless steel
columns.
C. Reagents
(a) Eluant.—Dilute mixture of 200 mL CH3CN (UV grade),
1.6 mL n-octyl amine, and 2.4 g (NH4)2HPO4 to 1 L with H2O
(0.4 mm filtered). Adjust pH of eluant to 7.0 with H3PO4. Eluant may
be recycled if reservoir is magnetically stirred and no more than
200 injections are made per L eluant.
(b) Dalapon standard solution.—130 mg/50 mL. Accurately
weigh ca 130 mg dalapon acid reference standard (99 +% isomer
pure; Dow Chemical Co.
mark, and shake. Do not use standard solution after 24 h. Determine
percent H2O in dalapon acid reference standard by Karl Fisher
titration. Labeled purity of reference standard is on anhydrous basis
and must be appropriately reduced according to water content.
D. Extraction of Analyte
Accurately weigh test portion containing ca 130 mg dalapon acid
equivalent into 50 mL beaker. Quantitatively transfer to 50 mL
volumetric flask with H2O. Fill to mark with H2O and shake. Do not
use test solution after 24 h. Dalapon acid and salts are hygroscopic;
protect from moisture in air by storing in well-sealed bottle. Prepare
test and standard solutions in duplicate. (Note: Do not add mineral
acids in extraction of analyte.)
E. Determination
Inject standard solution, test solution, and then standard solution.
Calculate results as
Dalapon acid equivalent, % = (R/R¢) ´ (W¢/W ´ P)
where R and R¢ = average peak height or peak area of dalapon peak for
test and standard solutions, respectively; W and W¢ = mg test portion
and standard, respectively; and P = percent purity of standard.
(Note: Initial system stability may be poor. Before injecting test
solution, repeat injection of standard solution to confirm system
stability. Periodically confirm linearity by analyzing standards
containing 100, 130, and 160 mg 99+% dalapon acid/50 mL H2O.
Flush injection loop with ³1 mL test or standard solution before
operating injection valve.)
References: JAOAC 66, 1390(1983); 70, 265(1987).
CAS 75-99-0 (dalapon)
ã 2005 AOAC INTERNATIONAL