使用Biotage Isolera快速纯化液相制备色谱进行川芎中洋川芎内酯A和Z藁本内酯的分离提取

The ethanolic extract of Aloe barbadensis Miller leaf skin showed inhibitory activity against phosphodiesterase-4D (PDE4D), which is a therapeutic target of inflammatory disease. Subsequent bioassay-guided fractionation led to the isolation of two new anthrones, 6′-Oacetyl- aloin B (9) and 6′-O-acetyl-aloin A (11), one new chromone, aloeresin K (8), together with thirteen known compounds. Their chemical structureswere elucidated by spectroscopic methods including UV, IR, 1D and 2DNMR, and HRMS. All of the isolateswere screened for their inhibitory activity against PDE4D using tritium-labeled adenosine 3′,5′-cyclic monophosphate (3H cAMP) as substrate. Compounds 13 and 14were identified as PDE4D inhibitors,with their IC50 values of 9.25 and 4.42μM, respectively. These achievements can provide evidences for the use of A. barbadensis leaf skin as functional feed additives for anti-inflammatory purpose.

Clandestine laboratories constantly produce new synthetic cannabinoids to circumvent legislative efforts,complicating toxicological analysis. No extensive synthetic cannabinoid quantitative urinary methodsare reported in the literature. We developed and validated a liquid chromatography–tandem mass spec-trometric (LC–MS/MS) method for simultaneously quantifying JWH-018, JWH-019, JWH-073, JWH-081,JWH-122, JWH 200, JWH-210, JWH-250, JWH-398, RCS-4, AM-2201, MAM-2201, UR-144, CP 47,497-C7,CP 47,497-C8 and their metabolites, and JWH-203, AM-694, RCS-8, XLR-11 and HU-210 parent com-pounds in urine. Non-chromatographically resolved alkyl hydroxy metabolite isomers were consideredsemi-quantitative.  Glucuronidase hydrolyzed urine was extracted with 1 ml Biotage SLE+ columns.Specimens were reconstituted in 150 L mobile phase consisting of 50% A (0.01% formic acid in water)and 50% B (0.01% formic acid in 50:50 methanol:acetonitrile). 4 and 25 L injections were performed toacquire data in positive and negative ionization modes, respectively. The LC–MS/MS instrument consistedof a Shimadzu UFLCxr system and an ABSciex 5500 Qtrap massspectrometer with an electrospray source.Gradient chromatographic separation was achieved utilizing a Restek Ultra Biphenyl column with a0.5 ml/min flow rate and an overall run time of 19.5 and 11.4 min for positive and negative mode methods,respectively. Quantification was by multiple reaction monitoring with CP 47,497 compounds and HU-210ionized via negative polarity; all other analytes were acquired in positive mode. Lower and upper limitsof linearity were 0.1–1.0 and 50–100 g/l (r2> 0.994).

Clandestine laboratories constantly produce new synthetic cannabinoids to circumvent legislative efforts,complicating toxicological analysis. No extensive synthetic cannabinoid quantitative urinary methodsare reported in the literature. We developed and validated a liquid chromatography–tandem mass spec-trometric (LC–MS/MS) method for simultaneously quantifying JWH-018, JWH-019, JWH-073, JWH-081,JWH-122, JWH 200, JWH-210, JWH-250, JWH-398, RCS-4, AM-2201, MAM-2201, UR-144, CP 47,497-C7,CP 47,497-C8 and their metabolites, and JWH-203, AM-694, RCS-8, XLR-11 and HU-210 parent com-pounds in urine. Non-chromatographically resolved alkyl hydroxy metabolite isomers were consideredsemi-quantitative.  Glucuronidase hydrolyzed urine was extracted with 1 ml Biotage SLE+ columns.Specimens were reconstituted in 150 L mobile phase consisting of 50% A (0.01% formic acid in water)and 50% B (0.01% formic acid in 50:50 methanol:acetonitrile). 4 and 25 L injections were performed toacquire data in positive and negative ionization modes, respectively. The LC–MS/MS instrument consistedof a Shimadzu UFLCxr system and an ABSciex 5500 Qtrap massspectrometer with an electrospray source.Gradient chromatographic separation was achieved utilizing a Restek Ultra Biphenyl column with a0.5 ml/min flow rate and an overall run time of 19.5 and 11.4 min for positive and negative mode methods,respectively. Quantification was by multiple reaction monitoring with CP 47,497 compounds and HU-210ionized via negative polarity; all other analytes were acquired in positive mode. Lower and upper limitsof linearity were 0.1–1.0 and 50–100 g/l (r2> 0.994).

1. 加热迅速，均匀。不需热传导过程，且具有自动热平稳性能，避免过热。 2. 加热质量高。营养破坏少，能最大限度的保持食物的色、香，味，减少食物中维生素的破坏。 3. 热惯性小。介质温升可无惰性的随之改变，不存在“余热”现象，极有利于自动控制和连续化生产的需要。 4. 安全卫生无污染。因为微波能是控制在金属制成的加热室内和波导管中工作，所以微波泄露被有效的抑制，没有放射线危害及有害气体排放，不产生余热和粉尘污染。 5. 节能高效。由于含有水分的物质极易直接吸收微波而发热，没有经过其他中间转换环节，因此除少量的传输损耗外几乎无其他损耗。比一般常规加热省电约30%～50%。