As the key point in sex hormone analysis, sample pre-treatment technology has attracted scientists' attention all over the world, and the development trend of sample preparation forwarded to faster and more efficient technologies. Taking economic and environmental concerns into account, subcritical fluid extraction as a faster and more efficient method has stood out as a sample pre-treatment technology. This new extraction technology can overcome the shortcomings of supercritical fluid and achieve higher extraction efficiency at relatively low pressures and temperatures. In this experiment, a simple, sensitive and efficient method has been developed for the determination of diethylstilbestrol(DES) in fish tissue using subcritical 1,1,1,2-tetrafluoroethane(R134a) extraction in combination with gas chromatography-mass spectrometry(GC-MS). After extraction, freezing-lipid filtration was utilized to remove fatty co-extract. Further purification steps were performed with C_(18) and NH_2 solid phase extraction(SPE). Finally, the analyte was derived by heptafluorobutyric anhydride(HFBA), followed by GC-MS analysis. Response surface methodology(RSM) was employed to optimizing the extraction condition, and the optimized was as follows: extraction pressure, 4.3 MPa; extraction temperature, 26℃; amount of co-solvent volume, 4.7 m L. Under this condition, at a spiked level of 1, 5, 10 μg kg~(-1), the mean recovery of DES was more than 90% with relative standard deviations(RSDs) less than 10%. Finally, the developed method has been successfully used to analyzing the real samples. 相似文献
Using Altera's Quartus Ⅱ, Nios Ⅱ IDE and Sopc Builder development tools, the proton precession magnetometer principle host hardware platform is designed in a cyclone Ⅱ series FPGA chip (EP2C35). The proton precession magnetometer principle host core circuit's single-chip system-logic design is achieved by building and configuring the Nios Ⅱ soft-core processor, developing the IO interface and sensor control circuits, programming some hardware units' VHDL code, for example the equal precision cymometer and the DPLL. Through researching the embedded operating system configuration technology and building the NIOS Ⅱ soft-core processor's μClinux cross-compile environment, the μClinux system is transplanted to the NIOS Ⅱ environment. Another important task is writing the device drivers' and user programs' code. Through these work, the design realize the host function and achieve the expected target.