title: Subzero-Temperature Liquid-Liquid Extraction Coupled with UPLC-MS-MS for the Simultaneous Determination of 12 Bioactive Components in Traditional Chinese Medicine Gegen-Qinlian Decoction.
abstract: Based on the phase separation phenomenon of acetonitrile-water system at subzero temperature, a subzero-temperature liquid-liquid extraction coupled with ultra-performance liquid chromatography tandem quadrupole mass spectrometry : UPLC-MS-MS) method was developed for the simultaneous determination of 12 bioactive components in Gegen-Qinlian decoction. After optimization, the extraction conditions were set as follows: 3.0 mL of aqueous sample solution (pH 5.86) was extracted with 2 mL of acetonitrile at -35°C for 35 min. The separated acetonitrile phase was diluted 10-fold with water before UPLC-MS-MS analysis. Separation was performed on a Waters ACQUITY UPLC(®)BEH C18 column (2.1 × 100 mm i.d., 1.7 µm) with ammonium formate buffer solution (20 mmol L(-1), pH 3.2, adjusted by formic acid) and acetonitrile as mobile phase with gradient elution. Twelve target components could be separated within 10 min and quantified in multiple reaction monitoring mode, both positive and negative ionization modes were employed. Limits of detection were in the range of 0.0003-0.0451 μg mL(-1). Relative standard deviation values for intra- and interday precision were <2.71 and 8.94%, respectively. The established method provides a simple and effective framework for the quality control of Gegen-Qinlian decoction and related traditional Chinese medicinal preparations.
authors: College of Chemistry and Environmental Science, Key Laboratory of Analytical Science and Technology of Hebei Province, Hebei University, Baoding 071002, China.
authors: Zhihong
authors: Z
authors: Shi
authors: College of Chemistry and Environmental Science, Key Laboratory of Analytical Science and Technology of Hebei Province, Hebei University, Baoding 071002, China.
authors: Zhimin
authors: Z
authors: Li
authors: College of Chemistry and Environmental Science, Key Laboratory of Analytical Science and Technology of Hebei Province, Hebei University, Baoding 071002, China.
authors: Shulan
authors: S
authors: Zhang
authors: College of Chemistry and Environmental Science, Key Laboratory of Analytical Science and Technology of Hebei Province, Hebei University, Baoding 071002, China.
authors: Hongna
authors: H
authors: Fu
authors: College of Chemistry and Environmental Science, Key Laboratory of Analytical Science and Technology of Hebei Province, Hebei University, Baoding 071002, China hyzhang@hbu.edu.cn.
authors: Hongyi
authors: H
authors: Zhang
mesh_terms: D000470:Alkaloids / Q000032:analysis* / Q000737:chemistry / Q000302:isolation & purification; D002851:Chromatography, High Pressure Liquid / Q000379:methods*; D003080:Cold Temperature; D004365:Drugs, Chinese Herbal / Q000737:chemistry*; D005419:Flavonoids / Q000032:analysis* / Q000737:chemistry / Q000302:isolation & purification; D057230:Limit of Detection; D016014:Linear Models; D059625:Liquid-Liquid Extraction / Q000379:methods*; D015203:Reproducibility of Results; D012503:Saponins / Q000032:analysis* / Q000737:chemistry / Q000302:isolation & purification; D053719:Tandem Mass Spectrometry / Q000379:methods
chemical_list: D000470:Alkaloids; D004365:Drugs, Chinese Herbal; D005419:Flavonoids; D012503:Saponins; C542794:gegenqinlian