以0.15 mol·L^-1硝酸溶液为提取溶剂超声提取植物样品2次，提取溶液经CNW IC-Guard RP小柱净化后，进入高效液相色谱，以Hamilton PRP-X100色谱柱为固定相，以25 mmol·L^-1磷酸氢二铵-甲酸溶液（pH 6.0）为流动相进行等度洗脱，分离其中的亚砷酸[As（Ⅲ）]、二甲基砷酸（DMA）、一甲基砷酸（MMA）和砷酸[As（Ⅴ）]，4种砷形态在9 min内可完全分离。将分离出的4种砷形态引入氢化物发生-原子荧光光谱仪进行测定，其中，硼氢化钾溶液（还原剂）的质量浓度为22.5 g·L^-1，盐酸溶液（载流）的浓度为1.2 mol·L^-1。结果表明：4种砷形态的质量浓度在5~100 μg·L^-1内与其对应的峰面积呈线性关系，检出限（3S/N）为0.20~0.46 μg·L^-1。采用标准加入法进行回收试验，得到回收率为80.0%~101%，测定值的相对标准偏差（n=6）为2.1%~5.0%。按此方法测定大米、芥菜、空心菜、莲藕、柑橘叶片等植物样品中的砷形态，均未检出MMA，检出As（Ⅲ）的质量分数（0.053~0.81 mg·kg^-1）相对较高，且该方法测得砷形态总和占按照GB 5009.11-2014测得总砷含量的百分比为84.2%~104%。

The plant sample was ultrasonically extracted with 0.15 mol·L^-1 nitric acid solution for 2 times. After centrifugation, the extraction solution was purified by the CNW IC-Guard RP column, then introduced into HPLC using Hamilton PRP-X100 chromatographic column as stationary phase and 25 mmol·L^-1 (NH₄)₂HPO₄-HCOOH solution(pH 6.0) as mobile phase in isocratic elution. The 4 species of arsenic (arsenite, dimethylated arsenic, monomethylated arsenic and arsenate) in sample solution were completely separated within 9 min, then the 4 species of arsenic were determined by HG-AFS with 22.5 g·L^-1 potassium borohydride solution as reductive agent and 1.2 mol·L^-1 hydrochloric acid solution as carrying current. The results showed that linearity relationships between peak area and mass concentration of the 4 species of arsenic were kept in the same range of 5-100 μg·L^-1, with detection limits (3S/N) in the range of 0.20-0.46 μg·L^-1. Values of recovery obtained by standard addition method were found in the range of 80.0% to 101%, and RSDs (n=6) of the measured values were found in the range of 2.1% to 5.0%. The proposed method was used for determination of plant samples including rice, mustard, swamp cabbage, lotus root, citrus leaves, and all of samples contained high mass fraction of arsenite (0.053-0.81 mg·kg^-1) while monomethylated arsenic was not detected, with percentage of the total arsenic species measured between this method and national standard method of GB 5009.11-2014 in the range of 84.2%-104%.