Page 40 - 理化检验-化学分册 2021年第六期

许珊珊, 等: 高效液相色谱 Ｇ 串联质谱法测定蔬菜中 ９ 种有机磷阻燃剂的含量

Determinationof９Or g ano p hos p horusFlameRetardantsinVe g etables
b yHi g hPerformanceLi q uidChromato g ra p h y Ｇ

Tandem MassS p ectrometr y

,
XUShanshan , SUN Wenfan g YANG Wen , LIUXian gp in g ∗
( Nan j in g Munici p alCenter f orDiseaseControlandPreventionA ff iliatedtoNan j in g
MedicalUniversit y , Nan j in g２１０００３ , China )

Abstract : A methodforthe determination of９ or g ano p hos p horusflameretardantsin ve g etables was
establishedb yhi g hp erformanceli q uidchromato g ra p h y Ｇtandem masss p ectrometr y ．TheQuEChERS method was
usedforsam p le p retreatment．Thesam p le ( ５．０g ) wasextractedwith１０mLofamixtureofacetonitrileandacetone
atvolumeratioof４∶１ , thewaterofwhichwereremoved , andtheanal y teswerep urified , blowntodr y nessb y
nitro g enandredissolvedwith０．５ mL methanol．Thechromato g ra p hicse p arationwasp erformedb yusin g Waters

ACQUITY UPLC BEH C １８ chromato g ra p hiccolumnasstationar yp hase , andthemixturesofa q ueoussolution
containin g０．１％ ( ) formicacidandmethanolsolutioncontainin g０．１％ ( ) formicacidatdifferentvolumeratios
φ
φ
＋
wereusedas mobilep haseforg radientelution．ESI andthe modeof multireaction monitorin g ( MRM ) were
ado p tedinMS / MS．Ionp airandretentiontimewereusedfor q ualitativeanal y sis , andexternalstandardmethodfor
q uantitativeanal y sis．Theresultsshowedthatlinearrelationshi p sofmassconcentrationsof９or g ano p hos p horus
－１
flameretardantswerefoundinthedefiniteran g es , withdetectionlimits ( ３S / N ) intheran g eof０．０１－１５ μ g k g ．
Testsforrecover yweremadeb y standardadditionmethod , g ivin g resultsintheran g eof６０．０％－１２０％ , andRSDs
ofthedeterminedvalues ( n＝５ ) alllessthan１０％．Thismethodwasusedtoanal y zethe７Ve g etablesam p les , and
thedetectionrateoftrieth y l p hos p hate ( TEP ) wasu p to１００％．
Ke y words : hi g h p erformanceli q uid chromato g ra p h y Ｇtandem mass s p ectrometr y ; QuEChERS method ;
or g ano p hos p horusflameretardant ; ve g etable

５ ０ ６