LAUSR

HIGHLIGHTSA UPLC‐MS/MS method was established for determination volatile in herb pair.Response surface analysis was employed to explain the herb–herb interactions.The results were positive to Cyperi Rhizoma herb pair based products development. ABSTRACT Cyperi Rhizoma (Xiangfu) combined with either Angelicae Sinensis Radix (Danggui) or Chuanxiong Rhizoma (Chuanxiong) are herb pairs that are commonly used in clinical settings. To illustrate the herb–herb interactions that occur when extracts from these herbs are obtained together, ultra‐high‐performance liquid chromatography coupled with triple quadrupole electrospray tandem mass spectrometry and response surface analysis were used. Volatile components, &agr;‐cyperone, nootkatone, ligustilide, senkyunolide A and senkyunolide I, were accurately identified with high precision. When Xiangfu was combined with Danggui at a 1:1 ratio, or with Chuanxiong at a 1:1 or 2:1 ratio, the dissolution rates of &agr;‐cyperone and nootkatone from the herbs were greatly increased, compared to those obtained from Xiangfu extract alone. The dissolution rates of ligustilide, senkyunolide A and senkyunolide I from Danggui or Chuanxiong changed proportionally to changes in the ratios of Xiangfu with either Danggui or Chuanxiong. Response surface analysis results presented polynomial regression equations between the dissolution of tested compounds and the corresponding input variables, including compatibility proportions and solvent dosage. Based on the predicted results from response surface analysis, a combination of Xiangfu with Chuanxiong at a ratio of near 1:1, or with Danggui at 1:2, resulted in the maximum dissolution of five volatile components. Our established method could be applied to herb–herb interaction research, and the results may provide a scientific basis for the development of Cyperi Rhizoma–Chuanxiong Rhizoma, or Cyperi Rhizoma–Angelicae Sinensis Radix‐based formulas and products.