PMID- 23518306 OWN - NLM STAT- MEDLINE DCOM- 20131112 LR - 20130429 IS - 1873-264X (Electronic) IS - 0731-7085 (Linking) VI - 80 DP - 2013 Jun TI - Qualitative and quantitative analysis of the major constituents in Chinese medicinal preparation Dan-Lou tablet by ultra high performance liquid chromatography/diode-array detector/quadrupole time-of-flight tandem mass spectrometry. PG - 50-62 LID - S0731-7085(13)00071-X [pii] LID - 10.1016/j.jpba.2013.02.011 [doi] AB - A rapid ultra high performance liquid chromatography/diode-array detector/quadrupole time-of-flight tandem mass spectrometry (UPLC-DAD-QTOF) method and a ultra high performance liquid chromatography coupled with diode-array detector (UPLC-DAD) method were developed for qualitative and quantitative analyses of the major chemical constituents in Dan-Lou tablet. Sixty-eight compounds including flavonoids, phenolic acids, tanshinones, protostane triterpenoids, lactones, and paeoniflorins were unambiguously or tentatively identified by comparing their retention times and accurate mass measurement in 40min with references or literature data. Among them, 19 compounds: gallic acid, danshensu, 5-hydroxymethyl-2-furaldehyde, 3'-hydroxy puerarin, puerarin, 3'-methoxy puerarin, mirificin, daidzin, paeoniflorin, calycosin-7-O-beta-D-glucoside, naringin, genistin, rosmarinic acid, salvianolic acid B, salvianolic acid A, formononetin, calycosin, cryptotanshinone and tanshinone IIA were further quantified in 30min as marker substances. It was found that the calibration curves for all analytes showed good linearity (R(2)>0.9997) within the test ranges. The overall limits of detection (LODs) and limits of quantification (LOQs) were 0.0073-0.34mug/mL and 0.022-1.04mug/mL, respectively. The relative standard deviations (RSDs) for intra- and inter-day precisions were below 1.90% and 2.85%, respectively. The results of repeatability were less than 2.74%. The sample was stable for at least 48h. The mean recovery rates ranged from 95.5% to 105% with the relative standard deviations (RSDs) less than 2.96%. The results showed that the developed quantitative method was linear, sensitive, and precise for quality control of Dan-Lou tablet. CI - Copyright (c) 2013 Elsevier B.V. All rights reserved. FAU - Dong, Juan AU - Dong J AD - Tianjin State Key Laboratory of Modern Chinese Medicine, Tianjin University of Traditional Chinese Medicine, Tianjin 300193, PR China. FAU - Zhu, Yan AU - Zhu Y FAU - Gao, Xiumei AU - Gao X FAU - Chang, Yanxu AU - Chang Y FAU - Wang, Meng AU - Wang M FAU - Zhang, Peng AU - Zhang P LA - eng PT - Journal Article PT - Research Support, Non-U.S. Gov't DEP - 20130227 PL - England TA - J Pharm Biomed Anal JT - Journal of pharmaceutical and biomedical analysis JID - 8309336 RN - 0 (Drugs, Chinese Herbal) RN - 0 (Tablets) SB - IM MH - Calibration MH - Chromatography, High Pressure Liquid/*methods MH - Drugs, Chinese Herbal/*analysis/chemistry MH - Limit of Detection MH - Quality Control MH - Reproducibility of Results MH - Sensitivity and Specificity MH - Tablets MH - Tandem Mass Spectrometry/*methods EDAT- 2013/03/23 06:00 MHDA- 2013/11/13 06:00 CRDT- 2013/03/23 06:00 PHST- 2012/10/26 00:00 [received] PHST- 2013/02/11 00:00 [revised] PHST- 2013/02/13 00:00 [accepted] PHST- 2013/03/23 06:00 [entrez] PHST- 2013/03/23 06:00 [pubmed] PHST- 2013/11/13 06:00 [medline] AID - S0731-7085(13)00071-X [pii] AID - 10.1016/j.jpba.2013.02.011 [doi] PST - ppublish SO - J Pharm Biomed Anal. 2013 Jun;80:50-62. doi: 10.1016/j.jpba.2013.02.011. Epub 2013 Feb 27.