Headspace single-drop microextraction coupled with gas chromatography electron capture detection of butanone derivative for determination of iodine in milk powder and urine

2013 ◽  
Vol 67 (10) ◽  
Author(s):  
Meihua Hu ◽  
Haiying Chen ◽  
Yong Jiang ◽  
Huifang Zhu

AbstractA new detection method using headspace single-drop microextraction (HS-SDME) coupled to gas chromatography (GC) was established to determine the iodine in milk powder and urine. The derivative from the reaction between iodine and butanone in the acidic media was extracted into a micro-drop then determined by GC-ECD. With the optimisation of HS-SDME and derivatisation, the calibration curve showed good linearity within the range of 0.004–0.1 μg mL−1 (0.004–0.1 μg g−1) (R 2 = 0.9991), and the limits of detection for milk powder and urine were 0.0018 μg g−1 and 0.36 μg L−1, respectively. The mean recoveries of milk powder and urine were 90.0–107 % and 89.4–101 % with mean RSD of 1.7–3.4 % and 2.7–3.3 %, respectively. This detection method affords a number of advantages, such as being simple, rapid, and inexpensive, with low organic solvent consumption, and is remarkably free from interference effects, rendering it an efficient method for the determination of iodine in milk powder and urine samples.

2013 ◽  
Vol 838-841 ◽  
pp. 2566-2569
Author(s):  
Jian Qi Sun ◽  
Bo Qiao ◽  
Jun Dai

This study describes an analytical method employing capillary gas chromatography (GC) using flame ionization detection (FID) that has been developed for the simultaneous determination of chlorobenzenes (m-dichlorobenzene (m-DCB),p-dichlorobenzene (p-DCB),o-dichlorobenzene (o-DCB) and 1,2,4-trichlorobenzene (1,2,4-TCB)) in wastewater. For this purpose, single-drop microextraction (SDME) was applied as a sample preparation technique. The SDME parameters such as types of extractants, volume of the microdroplet size, extraction time, stir rate and immersion depth of needle point were studyed and optimized. The method was linear in the ranges from 4.0×10-3to 40.0 μg·mL-1form-DCB,p-DCB ando-DCB, and 4.0×10-3to 30.0 μg·mL-1for 1,2,4-TCB withR2≥0.9955. The SDME procedure allowed efficient recovery of the investigated chlorobenzenes ranging between 80 % and 105 % with a relative standard deviation (RSD) ≤6.5 for actual wastewater sampes spiked with 2, 5 and 10 μg·mL-1of chlorobenzes, respectively. These results showed the potential of this technique for chlorobenzenes monitoring in wastewater samples. Furthermore, the investigated methods are simple, reliable, reproducible, and not expensive.


2013 ◽  
Vol 295-298 ◽  
pp. 487-491
Author(s):  
Jian Qi Sun

Single-drop microextraction (SDME) coupled to capillary gas chromatography (GC) was established for the determination of seven volatile halogenated hydrocarbons in wastewater, including chloroform (CF), carbon tetrachloride (CT), trichloroethylene (TCE), bromodichloromethane (BDCM), perchlorethylene (PCE), dibromochloromethane (DBCM) and bromoform (BF). The SDME parameters such as extractants, extracting time,stirring rate and immerging depth of needle point were studyed and optimized. The abovementioned halogenated hydrocarbons were quantified by external standardization method using GC coupled with a flame ionization detector (FID). The linear regression calibration curves, detection limits (S/N=3) and the linear ranges of the method for determining each halogenated hydrocarbons were determined, respectively. The concentrations of componds abovementioned in a real wastewater sample, the average of the recoveries obtained in the spiked wastewater samples and the corresponding relative standard deviations were determined, respectively. The results showed the proposed method several attributes, friendly enviroment, economic and highly efficient pretreatment, less time, simplicity, sensitivity, accuracy and wide linear range and so on.


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