TY - JOUR
T1 - Determination of aqueous fullerene aggregates in water by ultrasound-assisted dispersive liquid-liquid microextraction with liquid chromatography-atmospheric pressure photoionization-tandem mass spectrometry
AU - Chen, Hsin Chang
AU - Ding, Wang Hsien
N1 - Funding Information:
This study was supported by a grant from the National Science Council of Taiwan under contract no. NSC 099-2811-M-008-066 . We also thank the Instrumental Center of National Central University for instrumental support.
PY - 2012/2/3
Y1 - 2012/2/3
N2 - A simple and solvent-minimized method for the determination of three aqueous fullerene aggregates (nC 60, nC 70, and aqueous [6,6]-phenyl C 61 butyric acid methyl ester (nPCBM)) in water samples is described. The method involves the use of ultrasound-assisted dispersive liquid-liquid microextraction (UA-DLLME) coupled liquid chromatography-tandem mass spectrometry with atmospheric pressure photoionization (LC-APPI-MS/MS). The parameters affecting the extraction efficiency of the analytes from water samples were systematically investigated and the conditions optimized. The best extraction conditions involved the rapid injection of a mixture of 1.0mL of 2-propanol (as a disperser solvent) and 10μL of benzyl bromide (as an extraction solvent) into 10mL of an aqueous solution (pH 10.0) containing 1% sodium chloride in a conical bottom glass tube. After ultrasonication for 1.0min and centrifugation at 5000rpm (10min), the sedimented phase 5.0μL was directly injected into the LC-APPI-MS/MS system. The limits of quantification (LOQs) were 150, 60 and 8ngL -1 for nPCBM, nC 60 and nC 70, respectively. The precision for these analytes, as indicated by relative standard deviations (RSDs), were less than 12% for both intra- and inter-day analysis. Accuracy, expressed as the mean extraction recovery, was between 70 and 86%. A standard addition method was used to quantitate three aqueous fullerene aggregates, and the concentrations of these aqueous fullerene aggregates were determined to be in the range from n.d. to 130ngL -1 in various environmental samples including municipal influent and effluent samples, industrial wastewater samples, and surface water samples.
AB - A simple and solvent-minimized method for the determination of three aqueous fullerene aggregates (nC 60, nC 70, and aqueous [6,6]-phenyl C 61 butyric acid methyl ester (nPCBM)) in water samples is described. The method involves the use of ultrasound-assisted dispersive liquid-liquid microextraction (UA-DLLME) coupled liquid chromatography-tandem mass spectrometry with atmospheric pressure photoionization (LC-APPI-MS/MS). The parameters affecting the extraction efficiency of the analytes from water samples were systematically investigated and the conditions optimized. The best extraction conditions involved the rapid injection of a mixture of 1.0mL of 2-propanol (as a disperser solvent) and 10μL of benzyl bromide (as an extraction solvent) into 10mL of an aqueous solution (pH 10.0) containing 1% sodium chloride in a conical bottom glass tube. After ultrasonication for 1.0min and centrifugation at 5000rpm (10min), the sedimented phase 5.0μL was directly injected into the LC-APPI-MS/MS system. The limits of quantification (LOQs) were 150, 60 and 8ngL -1 for nPCBM, nC 60 and nC 70, respectively. The precision for these analytes, as indicated by relative standard deviations (RSDs), were less than 12% for both intra- and inter-day analysis. Accuracy, expressed as the mean extraction recovery, was between 70 and 86%. A standard addition method was used to quantitate three aqueous fullerene aggregates, and the concentrations of these aqueous fullerene aggregates were determined to be in the range from n.d. to 130ngL -1 in various environmental samples including municipal influent and effluent samples, industrial wastewater samples, and surface water samples.
KW - APPI
KW - Aqueous fullerene aggregates
KW - LC-MS
KW - Ultrasound-assisted dispersive liquid-liquid microextraction
KW - Water analysis
UR - http://www.scopus.com/inward/record.url?scp=84855850819&partnerID=8YFLogxK
U2 - 10.1016/j.chroma.2011.12.034
DO - 10.1016/j.chroma.2011.12.034
M3 - 期刊論文
C2 - 22209304
AN - SCOPUS:84855850819
SN - 0021-9673
VL - 1223
SP - 15
EP - 23
JO - Journal of Chromatography A
JF - Journal of Chromatography A
ER -