作者：苗雪雪¹, 龚浩如¹, 陶曙华¹, 陈英姿¹, 陈祖武¹, 刘登彪²

作者单位：1. 湖南省农业科学院水稻研究所, 湖南 长沙 410125;
2. 航天凯天环保科技股份有限公司, 湖南 长沙 410125

关键词：微波消解;钼锑抗比色法;蔬菜;总磷

摘要：

采用微波消解-钼锑抗光度法测定蔬菜中的总磷，为获得最佳试验条件，对微波消解条件中的酸的种类、消解时间和消解温度等影响因素进行优化，结果表明：硝酸和过氧化氢（体积比7∶1）为最佳消解酸系，最高消解温度180℃，保持时间20 min。对紫外-可见光波长和显色时间对试验结果的影响进行探讨，结果表明710 nm和20 min为最佳试验条件。为评价该方法的可靠性，选用两种蔬菜标准物质GBW 10048和GBW 10049对该方法进行分析验证，测定值与标准值相符，相对标准偏差（RSD）分别为0.884%和0.938%，添加回收率大于89.93%，表明该方法拥有良好的准确性和精密度。微波消解-钼锑抗光度法具有简单、省时省力、试剂用量少等优点，能够满足蔬菜中总磷的测定。

Microwave digestion combined with molybdenum antimony resistance spectrophotometric method for the determination of total phosphorus in vegetables

MIAO Xuexue¹, GONG Haoru¹, TAO Shuhua¹, CHEN Yingzi¹, CHEN Zuwu¹, LIU Dengbiao²

1. Hunan Rice Research Institute, Hunan Academy of Agricultural Sciences, Changsha 410125, China;
2. China Aerospace Kaitian Environmental Technology Co., Ltd., Changsha 410125, China

Abstract: A microwave digestion combined with molybdenum-antimony anti-spectrophotometric method is used for the determination of total phosphorus in vegetables. To get optimum test conditions, the parameters affecting the microwave digestion such as acid types, digestion time and temperature are optimized. Results show that HNO₃ and H₂O₂(7:1,ν/ν) are the best digestive acids, the digestion temperature is 180℃ and the time is 20 min. The effects of ultraviolet-visible wavelength and developing time on the test results are discussed and results show that 710 nm and 20 min are the optimum conditions. To evaluate the reliability of the method, two types of vegetable reference materials GBW 10048 and GBW 10049 are used for the analysis and verification of the method. Results show that tested values are in agreement with standard values, the relative standard deviation(RSD) is 0.884% and 0.938% and the fortified recovery is higher than 89.93%, showing the method has good accuracy and precision. Compared with the traditional method, the microwave digestion combined with molybdenum-antimony anti-spectrophotometric method is simple, rapid and environment-friendly and the method is suitable for the determination of total phosphorus in vegetables.

Keywords: microwave digestion;molybdenum antimony resistance colorimetric;vegetables;total phosphorus

2017, 43(12): 45-49  收稿日期: 2017-03-23;收到修改稿日期: 2017-05-19

基金项目: 

作者简介: 苗雪雪(1989-),女,河南安阳市人,研究实习员,硕士,主要从事农产品质量分析和农药残留分析研究。

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