Chlorophenols (CPs) exist in waste water of chemical and paper-making industries. Most of CPs with strong toxicity are difficult to be biodegraded, and can accumulate in organisms. Therefore, CPs have been listed as one of main organic pollutants by EPA of America. This paper conducts the sample pretreatment to five kinds of CPs in river water by Qdaura® Automatic SPE System, and compares it with the manual pretreatment method.
SPE Cartridge: Cleanert® PEP (500 mg / 6 mL)
Adjust the pH of 500 mL of water sample with 0.5 mol/L H2SO4 to 1.5~2.0.
Activation: activate the PEP cartridge with 5 mL of methanol and 5 mL of water sequentially.
Sample loading: load water sample onto the cartridge at a flow rate of below 5 mL/min.
Washing: Wash the cartridge with 5 mL of pure water and dry the cartridge under nitrogen stream for 20 min. Wash the cartridge with 0.8 mL of methanol (stand for 2 min to ensure methanol to soak packing material thoroughly) and discard the eluate.
Elution: Elute the cartridge with 5 mL of furanidine. Collect the eluate and concentrate under nitrogen stream at 30 °C to 1 mL for HPLC determination.
Column: Unisol C18, 4.6 mm × 150 mm, 5 μm, 100 Å
Mobile phase: A, water with 0.1% formic acid; B, methanol with 0.1% formic acid
Injection: 20 μL
Temperature: 30 °C
Detection UV: 285 nm
Table 1 Gradient Elution Condition
Flow rate (mL/min)
Results and Discussion
Table 2 Recoveries and reproducibility of spiked water sample (n=3, 1 μg/L)
Figure 1 Chromatogram of spiked water sample (1 μg/L)
It is shown by the test results that the recovery and RSD of spiked samples from river water through the sample pretreatment by a full-automatic solid-phase extractor are significantly superior to those through the manual solid-phase extraction.
500 mg / 6 mL
Qdaura® Automatic SPE System
4 channels, 24 positions