The invention discloses a quantitative detection kit combining magnetic particles with chemiluminescence immunoassay for angiotensin (Ang) I. The kit comprises Ang I calibrators, magnetic particle suspension coupled with streptavidin, an Ang I antibody labeled with biotin, an Ang I enzyme combination, an Ang I quality controller, chemiluminescence liquor A, chemiluminescence liquor B, 20 times concentrated washing liquor, and a reaction tube, wherein enzyme adopted by the Ang I enzyme combination is horse radish peroxidase with the purity RZ being more than or equal to 3.0 and the activity being more than or equal to 250U/ml. The invention also discloses a preparation method of the kit. Compared with the conventional kit, the quantitative detection kit is simple and convenient to operate, is safe, does not cause environment pollution, and also has the advantages of wide concentration range, low cost, good stability and the like of detection samples.