title: Comparison of two extraction methods for the determination of 135 pesticides in Corydalis Rhizoma, Chuanxiong Rhizoma and Angelicae Sinensis Radix by liquid chromatography-triple quadrupole-mass spectrometry. Application to the roots and rhizomes of Chinese herbal medicines.
abstract: In this study, two simple pretreatment methods were comprehensively evaluated for the determination of 135 pesticide residues in roots and rhizomes of Chinese herbal medicines (CHMs). The studied methodologies are (a) solid-phase extraction (SPE) and (b) Quick, Easy, Cheap, Effective, Rugged and Safe (QuEChERS). For SPE, extraction solvents, SPE cartridges and types and volume of eluent were accessed and optimized. For QuEChERS, different versions, acetic acid concentration and dispersive solid-phase extraction (dSPE) sorbent materials were tested. SPE and QuEChERS were estimated in recovery range, the number of pesticides that were recovered ranging from 90% to 110% and expenses in Corydalis Rhizoma, Chuanxiong Rhizoma and Angelicae Sinensis Radix. QuEChERS method showed better performance than SPE. The method showed good linearity over the range assayed 0.9986-0.9999 (1-80ng/mL for 124 pesticides, 1-50ng/mL for 10 pesticides, 1-20ng/mL for satisfar). The matrix effect was compensated by matrix-based calibration curves with internal standard. The average recoveries of all pesticides were ranging from 70% to 120% at three levels of 10, 50 and 100ng/g with relative standard deviations less than 20%. The limits of quantification of the 135 pesticides in three matrices were 1-5ng/g, which were below the maximum residue levels (MRLs) established by the European Union. The verified QuEChERS method was successfully applied to the analysis of 65 actual samples from eight different types of roots and rhizomes of CHMs. Angelicae Sinensis Radix was the most susceptible to pesticides among these samples, and the most frequently detected pesticide was carbendazim with levels below MRLs. Metalaxyl, phorate, atrazine, diniconazole, coumaphos and paclobutrazol were also detected in some samples.
authors.affiliation: School of Pharmacy, Shenyang Pharmaceutical University, 103 Wenhua Road, Shenhe District, Shenyang 110016, China; Pharmaceutical Analysis Institute, Tasly Holding Group Academy, Tianjin 300402, China.
authors.forename: Jie
authors.initials: J
authors.lastname: Liu
authors.affiliation: Pharmaceutical Analysis Institute, Tasly Holding Group Academy, Tianjin 300402, China.
authors.forename: Ling
authors.initials: L
authors.lastname: Tong
authors.affiliation: Pharmaceutical Analysis Institute, Tasly Holding Group Academy, Tianjin 300402, China.
authors.forename: Dongxiang
authors.initials: D
authors.lastname: Li
authors.affiliation: Pharmaceutical Analysis Institute, Tasly Holding Group Academy, Tianjin 300402, China.
authors.forename: Wenting
authors.initials: W
authors.lastname: Meng
authors.affiliation: School of Pharmacy, Shenyang Pharmaceutical University, 103 Wenhua Road, Shenhe District, Shenyang 110016, China; Pharmaceutical Analysis Institute, Tasly Holding Group Academy, Tianjin 300402, China.
authors.forename: Wanyang
authors.initials: W
authors.lastname: Sun
authors.affiliation: School of Pharmacy, Shenyang Pharmaceutical University, 103 Wenhua Road, Shenhe District, Shenyang 110016, China. Electronic address: yunli76@163.com.
authors.forename: Yunli
authors.initials: Y
authors.lastname: Zhao
authors.affiliation: School of Pharmacy, Shenyang Pharmaceutical University, 103 Wenhua Road, Shenhe District, Shenyang 110016, China. Electronic address: zhiguo-yu@163.com.
authors.forename: Zhiguo
authors.initials: Z
authors.lastname: Yu
mesh_terms: D002138:Calibration; D002853:Chromatography, Liquid / Q000379:methods*; D057230:Limit of Detection; D013058:Mass Spectrometry / Q000379:methods*; D010573:Pesticide Residues / Q000032:analysis*; D018517:Plant Roots / Q000737:chemistry; D015203:Reproducibility of Results; D027343:Rhizome / Q000737:chemistry*
chemical_list: D010573:Pesticide Residues
keywords: Chinese herbal medicines; Pesticides; QuEChERS; Solid-phase extraction; UHPLC–MS/MS