CAJ | 학술논문

目的：应用高效液相色谱(HPLC)和电感耦合等离子体质谱(ICP-MS)联用技术优化完善不同膳食基质中五价砷(As5+)、砷甜菜碱(AsB)、三价砷(As3+)、二甲基砷酸(DMA)和一甲基砷酸(MMA)5种砷形态的检测方法。方法通过比较不同浓度的乙酸、盐酸、硝酸水溶液在热提取条件下对不同膳食基质(谷类、饮料类、水产类、蛋类、豆类、水果类、糖类)及对NIST标准参考物质Rice Flour1568b中5种砷形态化合物的提取效果,确定最佳提取试剂和最佳提取浓度,同时比较不同 pH、不同流动相下砷化合物的分离效果,确定最终分离条件。结果膳食样品中砷形态分析的最佳提取方法为0.15 mol/L硝酸水溶液浸泡提取；以20 mmol/L柠檬酸和5 mmol/L己烷磺酸钠的混合溶液为流动相(pH=4.3),5种砷形态的线性范围线0~100μg/L相关系数(r)均大于0.999,检出限为0.4~1.2μg/L,精密度好, RSD均小于5%。不同膳食样品(谷类、饮料类、水产类、蛋类、豆类、水果类、糖类)加标回收率为80%~113%(无机砷)、81%~122%(MMA)、80%~124%(DMA)、77%~121%(AsB)；采用本方法测定的NIST标准参考物质Rice Flour 1568b测定值跟标示值相吻合。结论本实验优化了砷形态分析的前处理方法和分离条件,不仅具有省时、快速高效,而且可以保证测定结果的准确性。
목적：응용고효액상색보(HPLC)화전감우합등리자체질보(ICP-MS)련용기술우화완선불동선식기질중오개신(As5+)、신첨채감(AsB)、삼개신(As3+)、이갑기신산(DMA)화일갑기신산(MMA)5충신형태적검측방법。방법통과비교불동농도적을산、염산、초산수용액재열제취조건하대불동선식기질(곡류、음료류、수산류、단류、두류、수과류、당류)급대NIST표준삼고물질Rice Flour1568b중5충신형태화합물적제취효과,학정최가제취시제화최가제취농도,동시비교불동 pH、불동류동상하신화합물적분리효과,학정최종분리조건。결과선식양품중신형태분석적최가제취방법위0.15 mol/L초산수용액침포제취；이20 mmol/L저몽산화5 mmol/L기완광산납적혼합용액위류동상(pH=4.3),5충신형태적선성범위선0~100μg/L상관계수(r)균대우0.999,검출한위0.4~1.2μg/L,정밀도호, RSD균소우5%。불동선식양품(곡류、음료류、수산류、단류、두류、수과류、당류)가표회수솔위80%~113%(무궤신)、81%~122%(MMA)、80%~124%(DMA)、77%~121%(AsB)；채용본방법측정적NIST표준삼고물질Rice Flour 1568b측정치근표시치상문합。결론본실험우화료신형태분석적전처리방법화분리조건,불부구유성시、쾌속고효,이차가이보증측정결과적준학성。
Objective To establish a method for detection and analysis 5 kinds of arsenic species, including As5+, AsB, As3+, DMA and MMA by using a high performance liquid chromatography (HPLC) and inductively coupled plasma mass spectrometry (ICP-MS) Methods The best extraction and concentration of reagents were determined by comparing the different concentrations of acetic acid, hydrochloric acid, and nitric acid solution under the condition of thermal extract of different dietary matrix (grains, drinks, aquatic products, eggs, beans, fruits and sugar) and the NIST standard reference material of 5 arsenic species in Rice Flour 1568b extraction effect. At the same time, different mobile phase separation effect was compared under different pH, arsenic compounds, the final separation conditions were determined. Results The best extraction method of arsenic speciation analysis in dietary samples was 0.15 mol/L nitric acid soak extract, with a mixture of 20 mmol/L citric acid and 5 mmol/L hexane sulfonic acid sodium solution as mobile phase (pH=4.3), it showed a good linearity within 0~100μg/L concentration of 5 different forms of arsenic (r>0.999), the detection limit was 0.4~1.2μg/L, which had a good precision, the relative standard deviation (RSD) was less than 5%and the standard addition recovery was 80%~113% (iAs), 81%~122% (MMA), 80%~124% (DMA), and 77%~121%(AsB). Using this method for determining the NIST standard reference material Rice Flour 1568 b measured value was consistent with marked value. Conclusion This experiment optimized the arsenic speciation analysis methods of pretreatment and separation conditions, it not only has the time-saving, fast and efficient, but also can ensure the accuracy of determination results.