A quick and nondestructive method using near-infrared(NIR) diffuse reflectance spectroscopy was presented for the determination of the contents of calycosin-7-glucoside and astragaloside in astragali radix. With liquid chromatograph/mass spectrometer analysis of the reference value, partial least squares method was applied to establish a quantitative analysis model on calycosin-7-glucoside and astragaloside. The results showed that the model of calycosin-7-glucoside had optimal performance with pretreatment method of multiplicative scatter correction, first derivative and Savitzky-Golay convolution smoothing. The determination coefficients was 0.826 6 whiel the root mean square prediction(RMSEP)was 0.022 7; determination coefficients of calibration set was 0.863 5 and the root mean square error of calibration (RMSEC) was 0.019 0. Astragaloside after second derivative and Savitzky-Golay convolution smoothing, the determination coefficients was 0.854 8, the root mean square prediction was 0.006 41; determination coefficients of calibration set was 0.796 3 and the root mean square error of calibration was 0.007 99. Studies have shown that near infrared spectroscopy combined with partial least squares method is rapid, reliable and it could be implemented in the content detection of Calycosin- 7- glucoside and astragaloside in Astragali Radix.In addition,In addition, through the analysis of Principal Component analysis,it can be found little difference between the regions of Gansu and non- Gansu, there will be higher degree of differentiation among Shanxi,Sichuan and Jilin after elimination the region of Gansu Astragalus.