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Enantioselective residue analysis of oxathiapiprolin and its metabolite in tea and other crops by ultra‐high performance liquid chromatography–tandem mass spectrometry
Author(s) -
Zhang Xinzhong,
Sun Hezhi,
Wang Xinru,
Li Hongxia,
Zhong Qing,
Luo Fengjian,
Chen Zongmao
Publication year - 2020
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.202000457
Subject(s) - chemistry , chromatography , tandem mass spectrometry , formic acid , ammonium acetate , residue (chemistry) , mass spectrometry , metabolite , enantiomer , elution , high performance liquid chromatography , organic chemistry , biochemistry
Oxathiapiprolin is the first chiral piperidinyl thiazole isoxazoline fungicide developed to control downy mildew and other diseases, and there were no prior reports on its enantiomeric residue. In this study, a modified quick, easy, cheap, effective, rugged, and safe extraction and purification method followed by ultra‐high performance liquid chromatography–tandem mass spectrometry determination was first developed and validated for the residue analysis of oxathiapiprolin enantiomers and its metabolite IN‐E8S72 in green tea and other crops. Oxathiapiprolin enantiomers and IN‐E8S72 were separated on a chiral Lux Cellulose‐3 column with the use of 0.1% formic acid in acetonitrile and 5 mmol/L ammonium acetate in water as mobile phases. IN‐E8S72 was eluted first, followed by (−)‐oxathiapiprolin, and then (+)‐oxathiapiprolin. The recoveries ranged from 53.3 to 125.3% with relative standard deviations ranging from 1.4 to 16.0%. The limits of quantification for (−)‐oxathiapiprolin and (+)‐oxathiapiprolin were 0.005 mg/kg in romaine lettuce, head cabbage, potato, grape, and garlic, 0.01 mg/kg in soybean and pea, and 0.025 mg/kg in green tea and dry pepper. The limits of quantification of IN‐E8S72 were twice those of (−)‐oxathiapiprolin. Screening results with real market samples indicated that there was no enantiomeric excess in the oxathiapiprolin residue in romaine lettuce.