CAJ | 학술논문

目的：测定14种海藻样品中总砷和无机砷的含量,同时分析样品中6种砷形态。方法将海藻样品经过微波消解的前处理方法,通过电感耦合等离子体质谱(inductively coupled plasma mass spectrometry, ICP-MS)测定总砷含量；根据国标方法中无机砷检测的前处理方法,通过原子荧光光谱(atomic fluorescence spectrometry, AFS)测定无机砷含量；最后通过酸提的前处理方法,利用高效液相色谱-氢化物发生-原子荧光光谱法(high performance liquid chromatography-ultraviolet photo-oxidation-hydride generation-atomic fluorescence spectrometry, HPLC-(UV)-HG-AFS)测定海藻样品中6种形态砷含量并与国标无机砷方法比较。结果14种海藻样品中总砷含量为0.038~46.2 mg/kg；无机砷含量为0.006~19.3 mg/kg；对HPLC-(UV)-HG-AFS仪器的优化和方法的摸索后,从海藻样品中主要测得的砷形态为As(III)、As(V)和DMA, MMA含量较少,没有测出AsB和 AsC。结论在砷形态较为复杂的海藻样品检测中,通过 HPLC-(UV)-HG-AFS 检测方法可以有效避免无机砷前处理中可能出现的有机砷向无机砷转变的现象,降低干扰,增加测试的准确性,更为具体地表现海藻样品中主要的砷形态含量。
목적：측정14충해조양품중총신화무궤신적함량,동시분석양품중6충신형태。방법장해조양품경과미파소해적전처리방법,통과전감우합등리자체질보(inductively coupled plasma mass spectrometry, ICP-MS)측정총신함량；근거국표방법중무궤신검측적전처리방법,통과원자형광광보(atomic fluorescence spectrometry, AFS)측정무궤신함량；최후통과산제적전처리방법,이용고효액상색보-경화물발생-원자형광광보법(high performance liquid chromatography-ultraviolet photo-oxidation-hydride generation-atomic fluorescence spectrometry, HPLC-(UV)-HG-AFS)측정해조양품중6충형태신함량병여국표무궤신방법비교。결과14충해조양품중총신함량위0.038~46.2 mg/kg；무궤신함량위0.006~19.3 mg/kg；대HPLC-(UV)-HG-AFS의기적우화화방법적모색후,종해조양품중주요측득적신형태위As(III)、As(V)화DMA, MMA함량교소,몰유측출AsB화 AsC。결론재신형태교위복잡적해조양품검측중,통과 HPLC-(UV)-HG-AFS 검측방법가이유효피면무궤신전처리중가능출현적유궤신향무궤신전변적현상,강저간우,증가측시적준학성,경위구체지표현해조양품중주요적신형태함량。
Objective The content of total arsenic and inorganic arsenic were determined in 14 seaweeds and 6 kinds of arsenic species were determined at the same time. Methods The content of total arsenic was determined by inductively coupled plasma mass spectrometry (ICP-MS) after microwave digestion. According to the pretreatment method of national standard method, the content of inorganic arsenic was determined by atomic fluorescence spectrometry (AFS). The results of 6 arsenic species were studied by high performance liquid chromatography-ultraviolet photo-oxidation-hydride generation-atomic fluorescence spectrometry (HPLC-(UV)-HG-AFS) after acid extraction, which were compared with the national standard method. Results In 14 seaweeds, the content of total arsenic ranged from 0.038 to 46.2 mg /kg and the content of inorganic arsenic ranged from 0.006 to 19.3 mg/kg. After the instrument optimization and methods of exploration, only As(III), As(V) and DMA were found in seaweed samples. The content of MMA was less. AsB and AsC were not detected. Conclusion Through the detection method of HPLC-(UV)-HG-AFS, some seaweed samples with complicated morphology can effectively avoid the transformation between organic arsenic and inorganic arsenic. It can reduce interference and increase the accuracy of the test. More arsenic speciation will be performed in seaweed samples.