Abstract��The quality control methods of standard addition test and quality control charts were introduced. According to the standard addition detection of malachite green and nitrofuran metabolites in primary aquatic products by LC/MS, the standard addition recoveries were analyzed. The quality control charts were drew by Origin, and the correlation of standard addition recoveries was analyzed by SPSS. The results indicated that the quality control charts could monitor the test results effectively, and they could ensure the detection results were accurate. The main reason which caused the variation of standard addition recycles was random error. The recoveries correlation between color malachite green and leuco malachite green was weak. The average standard addition recycles of leuco malachite green was higher than that of color malachite green. In four kinds of nitrofuran metabolites, the recoveries correlation between AOZ and AMOZ or SEM was better than others. The average standard addition recycles of AOZ was maximum, and the average standard addition recycles of SEM was minimum.