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Solid‐phase extraction and residue determination of glyphosate in apple by ion‐pairing reverse‐phase liquid chromatography with pre‐column derivatization
Author(s) -
Qian Kun,
Tang Tao,
Shi Tianyu,
Li Pingliang,
Li Jianqiang,
Cao Yongsong
Publication year - 2009
Publication title -
journal of separation science
Language(s) - English
Resource type - Journals
SCImago Journal Rank - 0.72
H-Index - 102
eISSN - 1615-9314
pISSN - 1615-9306
DOI - 10.1002/jssc.200900118
Subject(s) - chromatography , derivatization , chemistry , solid phase extraction , residue (chemistry) , glyphosate , reversed phase chromatography , high performance liquid chromatography , extraction (chemistry) , organic chemistry , agronomy , biology
A new method for glyphosate residue determination in apple has been developed. A SPE cartridge was used to clean up the samples before derivatization. Glyphosate was derivatized with 4‐chloro‐3,5‐dinitrobenzotrifluoride (CNBF) and quantified by reverse ion‐pair liquid chromatography using cetyltrimethylammonium bromide (CTAB) as ion‐pair reagent. In pH 9.5 H 3 BO 3 –Na 2 B 4 O 7 medium, the reaction of glyphosate with CNBF was complete after 30 min at 60°C. The stability of the derivative on exposure to light at room temperature in methanol–water was demonstrated. The labeled glyphosate was separated on a Kromasil C 18 column (250×4.6 mm, 5 μm) at room temperature and UV detection was applied at 360 nm. Separation was achieved within 15 min in gradient elution mode. The correlation coefficient for the method was 0.9998 at concentrations ranging from 0.1 to 50 μg/g. The calculated recoveries for glyphosate in apple were from 86.00 to 99.55%, and the relative standard deviations ( n = 6) were from 1.43 to 6.32. The limit of detection was 0.01 μg/g for glyphosate in apple.