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重复两次。萃取液合并，用甲醇稀释至4.0 mL。溶液过0.45µm 滤膜备用。
加标浓度为1.0 和20 ng/mL
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Procedure for determination of phloxine B coffee bean samples
the GO-MISPE monolithic capillary column 1.分别用100μl甲醇和水活化
Analytica Chimica Acta
Impact Factor: 4.517
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Introduction
Phloxine B an insecticide
gastric toxicity and cell toxicity detect：HPLC CZE
SPE
MIPs high selectivity and specific recognition
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Preparation of phloxine B coffee bean samples
The sample solutions
咖啡豆研磨后过 20 目筛，转移至广口瓶于5 0C保存。
咖啡豆粉末(1.0 g)
2.0mL 甲醇萃取
离心
phloxine B 标准溶液 超声15 min 10,000 rpm,10 min
活化
2.样品溶液以0.02ml/min流速通过毛细管整体柱
进样
3.用40μl甲苯以0.02ml/min流速洗涤
去除杂质
4.用40μl 甲醇-乙酸(90:10, v/v) 0.1 mL/ min洗脱
洗脱
收集洗脱液，氮气吹干，残留物溶解于0.2ml甲醇 HPLC–LIF
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Results and discຫໍສະໝຸດ Baidussion
• Methanol
augmented the solubility of GO and phloxine B
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T:M:C
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Capacity of the column
capacity
0.006μg/mg 0.029μg/mg 0.040μg/mg 0.012μg/mg
Fig. 4.Breakthrough curves of phloxine B on GO-NIPs, MIPs and GO-MIPs column and breakthrough
curves of rose bengal on GO-MIPs column. Loading concentration: 1.0mg/mL; Sample flow rate: 0.02 mL/ min
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Fig. 3.FT-IR spectra of (a) GO and (b) GO-MIPs.
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porogen
methanol–toluene–dodecanol
permeable ,the flow rate of 0.15 ml/min
• toluene and dodecanol
30–40% keep the pore size voidless structure
porogen GO methanol
toluene
ultrasonication
30min
mechanically stirred
dodecanol
phloxine B (template) 1h,room temperature
MAA(functional monomer)
EDMA (crosslinker)
column
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Preparation of the GO-MISPE monolithic capillary column
The corresponding GO-NIPs monolithic capillary column --without template MIPs monolithic capillary column--without GO
Molecularly imprinted coated graphene oxide solid-phase extraction monolithic capillary column for selective extraction and sensitive determination of phloxine B in coffee bean
GO-MIPs higher loading capacity
faster association/dissociation kinetics improving the accessibility and sensitivity to target species 2
Preparation of the GO-MISPE monolithic capillary column
physicochemical stability and applicability
MISPE
MISPE monolithic column higher chemical stability,selectivity
more facile preparation
Preparation: in situ polymerization using nanostructured imprinted materials－GO
Fig. 1. The chemical structure of phloxine B.
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Synthesis and morphology
Fig. 2.SEM images of (a) the column prepared with AM, (b) the column prepared with MAA, (c) MIPs, (d) GO-MIPs and (e) the magnification is 20,000 folds for d
AIBN (initiator) purged with N2
5min
fill
(capillary tube)
polymerization,5h
wash
60 oC in a water-bath 甲醇-乙酸 (90:10, v/v)
wash the GO-MISPE methanol monolithic capillary