The present study was designed to develop and validate a sensitive and reliable ultra high performance liquid chromatography coupled with quadrupole time-of-flight mass spectrometry(UPLC-QTOF/MS) method to separate an...The present study was designed to develop and validate a sensitive and reliable ultra high performance liquid chromatography coupled with quadrupole time-of-flight mass spectrometry(UPLC-QTOF/MS) method to separate and identify the chemical constituents of Qixue Shuangbu Tincture(QXSBT), a classic traditional Chinese medicine(TCM) prescription. Under the optimized UPLC and QTOF/MS conditions, 56 components in QXSBT, including chalcones, triterpenoids, protopanaxatriol, flavones and flavanones were identified and tentatively characterized within a running time of 42 min. The components were identified by comparing the retention times, accurate mass, and mass spectrometric fragmentation characteristic ions, and matching empirical molecular formula with that of the published compounds. In conclusion, the established UPLC-QTOF/MS method was reliable for a rapid identification of complicated components in the TCM prescriptions.展开更多
Thirteen kinds of steroid hormones in raw milk（cow, goat and buffalo milk） were analyzed with ultra performance liquid chromatography-quadrupole time of flight mass spectrometry（UPLC-QTOF-MS） after extraction and ...Thirteen kinds of steroid hormones in raw milk（cow, goat and buffalo milk） were analyzed with ultra performance liquid chromatography-quadrupole time of flight mass spectrometry（UPLC-QTOF-MS） after extraction and cleanup with the modified Qu ECh ERS method. These steroid hormones included 17β-estradiol, estriol, estrone, diethylstilbestrol, progesterone, melengestrol acetate, megestrol acetate, chlormadinone acetate, 19-nortestosterone, metandienone, boldenone, epitestosterone, and testosterone. The limits of detection for the raw milk basing on 3 times the signal to noise ratios（S/N=3） was in range of 0.07-0.51 μg kg^–1, and the limits of quantification（basing on S/N=10 method） covered the ranges from 0.23 to 1.7 μg kg^–1. With matrix external standard method, the substances presented recoveries over the range 74.2–99.7%. Qualitative analysis was also done in the mass/mass spectrum（MS/MS） mode and each debris structure of 13 kinds of steroid hormones was achieved. The methodology was then applied in real raw milk samples which were collected in several areas of China and the progesterone was detected with high level.展开更多
Astragali Radix, the root of Astragalus membranaceus(Fisch.) Bge. var. mongholicus(Bge.) Hsiao or Astragalus membranaceus(Fisch.) Bge., is widely used as a tonic decoction pieces in the clinic of traditional Chinese m...Astragali Radix, the root of Astragalus membranaceus(Fisch.) Bge. var. mongholicus(Bge.) Hsiao or Astragalus membranaceus(Fisch.) Bge., is widely used as a tonic decoction pieces in the clinic of traditional Chinese medicine(TCM). Astragali Radix has various processed products with varying pharmacological actions. There is no modern scientific evidence to explain the differences in pharmacological activities and related mechanisms. In the present study, we explore the changes in chemical components in Astragali Radix after processing, by ultra-high performance liquid chromatography quadrupole time-of-flight mass spectrometry(UPLC-QTOF-MS) combined with novel informatics UNIFI platform and multivariate statistical analysis. Our results showed that the crude and various processed products could be clearly separated in PCA scores plot and 15 significant markers could be used to distinguish crude and various processed products by OPLS-DA in UNIFI platform. In conclusion, the present study provided a basis of chemical components for revealing connotation of different processing techniques on Astragali Radix.展开更多
目的建立桂枝茯苓胶囊（GFC）三萜类成分UPLC指纹图谱方法,为评价GFC的质量提供新方法。方法采用Agilent Zorbox Eclipse Plus HD C18（100 mm×2.1 mm,1.8μm）色谱柱,以乙腈-0.1%磷酸水溶液为流动相,梯度洗脱,体积流量0.2 m L/min...目的建立桂枝茯苓胶囊（GFC）三萜类成分UPLC指纹图谱方法,为评价GFC的质量提供新方法。方法采用Agilent Zorbox Eclipse Plus HD C18（100 mm×2.1 mm,1.8μm）色谱柱,以乙腈-0.1%磷酸水溶液为流动相,梯度洗脱,体积流量0.2 m L/min,柱温30℃,检测波长为210 nm。采用Q-TOF/MS对指纹图谱中共有峰进行指认。结果得到分离度和重复性良好的GFC三萜类成分指纹图谱,确定了20个共有峰,其中1-7、10、12、14-17号峰共13个共有峰来自于茯苓,8、11号峰来自于桂枝,9号峰来自于白芍和牡丹皮,13号峰来自于桃仁、白芍、牡丹皮和桂枝。10批成品指纹图谱相似度在0.90以上。UPLC-Q-TOF/MS共鉴定出15个成分,分别为常春藤皂苷（1）、去氢土莫酸（2）、土莫酸（3）、猪苓酸C（4）、3-表去氢土莫酸（6）、茯苓酸D（7）、α-亚麻酸（9）、去氢茯苓酸（10）、齐墩果酸（11）、茯苓酸（12）、亚油酸（13）、棕榈油酸甲酯（15）、棕榈酸（16）、棕榈酸乙酯（17）、胡萝卜苷（18）。结论建立的UPLC指纹图谱有较好的精密度、重复性和稳定性,适用于GFC的质量控制。展开更多
基金supported by the Natural Science Fund Project in Jiangsu Province,China(No.BK20141093)Jiangsu Province Science and Technology Support Plan-Industrial Projects(No.BE2012011)
文摘The present study was designed to develop and validate a sensitive and reliable ultra high performance liquid chromatography coupled with quadrupole time-of-flight mass spectrometry(UPLC-QTOF/MS) method to separate and identify the chemical constituents of Qixue Shuangbu Tincture(QXSBT), a classic traditional Chinese medicine(TCM) prescription. Under the optimized UPLC and QTOF/MS conditions, 56 components in QXSBT, including chalcones, triterpenoids, protopanaxatriol, flavones and flavanones were identified and tentatively characterized within a running time of 42 min. The components were identified by comparing the retention times, accurate mass, and mass spectrometric fragmentation characteristic ions, and matching empirical molecular formula with that of the published compounds. In conclusion, the established UPLC-QTOF/MS method was reliable for a rapid identification of complicated components in the TCM prescriptions.
基金supported by the Natural Science Foundation of Shandong Province,China(ZR2015CM015)the Special Fund for Agro-Scientific Research in the Public Interest,China(201403071)
文摘Thirteen kinds of steroid hormones in raw milk（cow, goat and buffalo milk） were analyzed with ultra performance liquid chromatography-quadrupole time of flight mass spectrometry（UPLC-QTOF-MS） after extraction and cleanup with the modified Qu ECh ERS method. These steroid hormones included 17β-estradiol, estriol, estrone, diethylstilbestrol, progesterone, melengestrol acetate, megestrol acetate, chlormadinone acetate, 19-nortestosterone, metandienone, boldenone, epitestosterone, and testosterone. The limits of detection for the raw milk basing on 3 times the signal to noise ratios（S/N=3） was in range of 0.07-0.51 μg kg^–1, and the limits of quantification（basing on S/N=10 method） covered the ranges from 0.23 to 1.7 μg kg^–1. With matrix external standard method, the substances presented recoveries over the range 74.2–99.7%. Qualitative analysis was also done in the mass/mass spectrum（MS/MS） mode and each debris structure of 13 kinds of steroid hormones was achieved. The methodology was then applied in real raw milk samples which were collected in several areas of China and the progesterone was detected with high level.
基金supported by the Construction Foundation of the State Administration of Traditional Chinese Medicine to the Processing Technology Heritage Base of TCM,Special Fund of the State Administration of Traditional Chinese Medicine to the Industry of TCM(No.20110700711)
文摘Astragali Radix, the root of Astragalus membranaceus(Fisch.) Bge. var. mongholicus(Bge.) Hsiao or Astragalus membranaceus(Fisch.) Bge., is widely used as a tonic decoction pieces in the clinic of traditional Chinese medicine(TCM). Astragali Radix has various processed products with varying pharmacological actions. There is no modern scientific evidence to explain the differences in pharmacological activities and related mechanisms. In the present study, we explore the changes in chemical components in Astragali Radix after processing, by ultra-high performance liquid chromatography quadrupole time-of-flight mass spectrometry(UPLC-QTOF-MS) combined with novel informatics UNIFI platform and multivariate statistical analysis. Our results showed that the crude and various processed products could be clearly separated in PCA scores plot and 15 significant markers could be used to distinguish crude and various processed products by OPLS-DA in UNIFI platform. In conclusion, the present study provided a basis of chemical components for revealing connotation of different processing techniques on Astragali Radix.
文摘目的建立桂枝茯苓胶囊（GFC）三萜类成分UPLC指纹图谱方法,为评价GFC的质量提供新方法。方法采用Agilent Zorbox Eclipse Plus HD C18（100 mm×2.1 mm,1.8μm）色谱柱,以乙腈-0.1%磷酸水溶液为流动相,梯度洗脱,体积流量0.2 m L/min,柱温30℃,检测波长为210 nm。采用Q-TOF/MS对指纹图谱中共有峰进行指认。结果得到分离度和重复性良好的GFC三萜类成分指纹图谱,确定了20个共有峰,其中1-7、10、12、14-17号峰共13个共有峰来自于茯苓,8、11号峰来自于桂枝,9号峰来自于白芍和牡丹皮,13号峰来自于桃仁、白芍、牡丹皮和桂枝。10批成品指纹图谱相似度在0.90以上。UPLC-Q-TOF/MS共鉴定出15个成分,分别为常春藤皂苷（1）、去氢土莫酸（2）、土莫酸（3）、猪苓酸C（4）、3-表去氢土莫酸（6）、茯苓酸D（7）、α-亚麻酸（9）、去氢茯苓酸（10）、齐墩果酸（11）、茯苓酸（12）、亚油酸（13）、棕榈油酸甲酯（15）、棕榈酸（16）、棕榈酸乙酯（17）、胡萝卜苷（18）。结论建立的UPLC指纹图谱有较好的精密度、重复性和稳定性,适用于GFC的质量控制。
