Study On Preparation Technology Of Organophosphrous Pesticides And Alkylphenols Referance Materials By High-performance Liquid Chromatography

Referance materials are used to calibrating equipment, evaluating measurement methodsor value assignments, and the separation and preparation technology of them is the focusresearch concerned by scholars. At present, the research level of referance materials in Chinais far behind the United States and other developed countries, the referance materials series ofenvironmental organic pollutants especially. It has seriously hampered the development ofenvironmental monitoring work. So it’s greatly necessary and urgent to accelerate researchand development of preparation technology of environmental organic pollutants referancematerials.This paper is supported by"The referance materials preparation of typical marine toxicorganic pollutants"(2006AA09Z164)which is one part of National863Plans Projects. Basedon the development status of environmental organic pollutants referance materials, referancematerials of five kinds of Organophosphrous pesticides(OPPs)、 bisphenol A and nonylphenol were separated and prepared by high-performance liquid chromatography(HPLC).And this paper also did some research to value these referance materials. The main researchresults are as follows:Under the conditions of210nm of UV wavelength、 methanol: water(70:30, v/v) asmobile phase, and flow rate of1.0mL/min, HPLC can separate five kinds of OPPs in theorginal liquid chemical products(omethoate, trichlorfon, dichlorvos, malathion, phorate). Theprecision is high. The minimum detection limits of the method range from1.05ng to42.72ng.Under the conditions of210nm of UV wavelength, flow rate of4.0mL/min and methanol:water(70:30, v/v) as mobile phase, five reference materials were prepared: the concentrationof omethoate is (725.41±3.87)μg/mL(purity=97.62%; V=1.64mL), the concentration oftrichlorfon is (3264.15±35.63)μg/mL(purity=98.40%; V=2.80mL), the concentration ofdichlorvos is (53.59±1.55)μg/mL(purity=99.39%; V=6.64mL), the concentration ofmalathion is (45.51±1.46)μg/mL(purity=99.45%; V=4.50mL), the concentration of phorate is(40.04±1.42)μg/mL(purity=99.66%; V=10.40mL). Develop HPLC methods to characterize reference materials of five kinds of OPPs. Repeatability is good. Their purity all achieverequirements of reference material.By F test, the uniformities of these five reference materials are good. In95%confidenceinterval, omethoate, trichlorfon, dichlorvos, malathion and phorate reference materials arestable under storage conditions of25℃,4℃and-25℃. It is recommended to storedichlorvos, malathion and phorate reference material below4℃.Under the conditions of210nm of UV wavelength, flow rate of4.0mL/min and methanol:water(90:10, v/v) as mobile phase, two reference materials were prepared: the concentrationof bisphenol A is (41.48±1.20)μg/mL(purity=97.62%; V=4.62mL), the concentration ofnonyl phenol is (74.20±1.06)μg/mL(purity=97.62%; V=3.48mL). Develop HPLC methods tocharacterize reference materials of bisphenol A and nonyl phenol. Repeatability is good. Theirpurity all achieve requirements of reference material.By F test, the uniformities of bisphenol A and nonyl phenol reference materials are good.In95%confidence interval, bisphenol A reference material is stable under storage conditionsof25℃,4℃and-25℃. It is recommended to store nonyl phenol reference material below4℃.