A simultaneous method was successfully established and validated for the separation and determination of bu- prenorphine （BP）, its primary metabolite, nor-buprenorphine （NBP） and a proposed co-formulate, naloxone ...A simultaneous method was successfully established and validated for the separation and determination of bu- prenorphine （BP）, its primary metabolite, nor-buprenorphine （NBP） and a proposed co-formulate, naloxone （NLX） in human plasma. The method used buprenorphine-d4 （BP-D4）, nor-buprenorphine-d3 （NBP-D3）, naltrexone （NTX） as internal standards （ISs）. 100 μL of plasma sample fortified with the ISs was cleaned up by solid-phase extraction （SPE）, and was then separated on a Waters AcquityTM BEH C18 column with gradient elution using methanol and water （containing 0.2% formic） at a flow rate of 0.25 mL·min^-1. The mass spectrometer was used for detection and was operated in the positive electrospray ionization with multiple reaction monitoring （MRM） mode. The three compounds were effectively separated in 5 min. The linear ranges of the compounds were 0.1--25, 0.25--25 and 0.05--25 ng·mL^-1 for BP, NBP and NLX, respectively, with r≥0.9935. The method had high sensitivity （the lim- its of detection were 0.02, 0.1 and 0.01 ng.mL-1 for BP, NBP and NLX, respectively） and high recoveries （≥97.6%）. The result was shown to be linear and satisfactorily met current acceptance criteria for validation of bio- analytical method： intra and inter assay precisions within the required limits of ≤25% RSD. The LOQs fulfilled the LOQ requirements： precision≤25% RSD, and was fully validated according to the State Food and Drug Administration （SFDA） regulations. The results demonstrated that ultra-high performance liquid chromatography- tandem mass spectrometer （UPLC-MS/MS） with SPE was a powerful detection tool and contributed to pharmaceutical analysis in biological matrices.展开更多
为建立铁皮石斛中2,4-表芸苔素内酯的高效、灵敏和准确的残留分析方法,利用超声与涡旋联用方法对铁皮石斛样品进行了提取,然后采用固相萃取小柱(Cleanert Pesti Carb/NH_(2))方法净化且经HPLC-MS/MS测定。经过方法学验证,2,4-表芸苔素...为建立铁皮石斛中2,4-表芸苔素内酯的高效、灵敏和准确的残留分析方法,利用超声与涡旋联用方法对铁皮石斛样品进行了提取,然后采用固相萃取小柱(Cleanert Pesti Carb/NH_(2))方法净化且经HPLC-MS/MS测定。经过方法学验证,2,4-表芸苔素内酯在铁皮石斛中的定量限和检出限分别为0.005 mg·kg^(-1)和0.0005 mg·L^(-1)。在0.005~0.5 mg·kg^(-1)的添加范围下,2,4-表芸苔素内酯在铁皮石斛中的平均回收率为94.70%~102.25%,相对标准偏差为1.3%~3.4%,表明该方法的灵敏度、准确度和精密度均满足铁皮石斛中2,4-表芸苔素内酯的农药残留分析要求。通过室内盆栽试验,获得了铁皮石斛样品,并利用该方法测定了铁皮石斛样品中2,4-表芸苔素内酯残留。2,4-表芸苔素内酯在铁皮石斛中的消解动态符合一级动力学,茎、叶半衰期分别为10.35~22.36 d和8.89~11.00 d,表明该方法能够应用于铁皮石斛实际样品的检测。展开更多
Ultra performance liquid chromatography(UPLC) coupled with orthogonal acceleration time-of-flight(oaTOF) mass spectrometry is becoming an effective and high-throughput analytical technique in metabonomics research.In ...Ultra performance liquid chromatography(UPLC) coupled with orthogonal acceleration time-of-flight(oaTOF) mass spectrometry is becoming an effective and high-throughput analytical technique in metabonomics research.In this paper,an UPLC-oaTOF-MS system was employed to investigate the serum profiles of 40 diabete mellitus(DM)/diabetic nephropathy(DN) patients and 25 healthy volunteers in an effort to find potential biomarkers.The UPLC system produced information-rich chromatograms with typical measured peak widths of 4 s,and generated peak capacities of 225 in 15 min.After the UPLC-oaTOF-MS analysis,principal component analysis(PCA) was used for group differentiation and marker selection.In the projection of positive mode,DM/DN patients and the controls were obviously divided into three groups.Furthermore,two potential markers were identified as phytosphingosine and sphinganine,respectively.Phytosphingosine and sphinganine with decreased concentrations in the patients,were closely related to the sphingolipid metabolism.展开更多
目的建立骨刺胶囊（昆布、骨碎补、白芍、党参等）指纹图谱,并结合质谱信息鉴定特征峰的化学结构信息。方法骨刺胶囊75%甲醇提取液的分析采用Phenomenex Luna C18柱（4.6 mm×250 mm,5μm）;流动相为乙腈-20 mmol/L甲酸铵水溶液体系...目的建立骨刺胶囊（昆布、骨碎补、白芍、党参等）指纹图谱,并结合质谱信息鉴定特征峰的化学结构信息。方法骨刺胶囊75%甲醇提取液的分析采用Phenomenex Luna C18柱（4.6 mm×250 mm,5μm）;流动相为乙腈-20 mmol/L甲酸铵水溶液体系;体积流量为1.0 m L/min,梯度洗脱;检测波长为254 nm。采用飞行时间质谱（TOFMS）结合离子阱多级质谱（Ion-trap/MSn）,鉴定骨刺胶囊指纹图谱中特征峰的结构,正、负两种离子模式扫描。结果骨刺胶囊HPLC-MS指认21个共有峰,表征昆布、白芍、杜仲、党参、马钱子、鸡血藤、骨碎补、延胡索和桂枝等9味药材的特征成分。以绿原酸为参照物峰,12批样品的相似度在0.821~0.945之间。结论该方法显示,骨刺胶囊主要化学成分相似,质量较稳定。展开更多
文摘A simultaneous method was successfully established and validated for the separation and determination of bu- prenorphine （BP）, its primary metabolite, nor-buprenorphine （NBP） and a proposed co-formulate, naloxone （NLX） in human plasma. The method used buprenorphine-d4 （BP-D4）, nor-buprenorphine-d3 （NBP-D3）, naltrexone （NTX） as internal standards （ISs）. 100 μL of plasma sample fortified with the ISs was cleaned up by solid-phase extraction （SPE）, and was then separated on a Waters AcquityTM BEH C18 column with gradient elution using methanol and water （containing 0.2% formic） at a flow rate of 0.25 mL·min^-1. The mass spectrometer was used for detection and was operated in the positive electrospray ionization with multiple reaction monitoring （MRM） mode. The three compounds were effectively separated in 5 min. The linear ranges of the compounds were 0.1--25, 0.25--25 and 0.05--25 ng·mL^-1 for BP, NBP and NLX, respectively, with r≥0.9935. The method had high sensitivity （the lim- its of detection were 0.02, 0.1 and 0.01 ng.mL-1 for BP, NBP and NLX, respectively） and high recoveries （≥97.6%）. The result was shown to be linear and satisfactorily met current acceptance criteria for validation of bio- analytical method： intra and inter assay precisions within the required limits of ≤25% RSD. The LOQs fulfilled the LOQ requirements： precision≤25% RSD, and was fully validated according to the State Food and Drug Administration （SFDA） regulations. The results demonstrated that ultra-high performance liquid chromatography- tandem mass spectrometer （UPLC-MS/MS） with SPE was a powerful detection tool and contributed to pharmaceutical analysis in biological matrices.
文摘Ultra performance liquid chromatography(UPLC) coupled with orthogonal acceleration time-of-flight(oaTOF) mass spectrometry is becoming an effective and high-throughput analytical technique in metabonomics research.In this paper,an UPLC-oaTOF-MS system was employed to investigate the serum profiles of 40 diabete mellitus(DM)/diabetic nephropathy(DN) patients and 25 healthy volunteers in an effort to find potential biomarkers.The UPLC system produced information-rich chromatograms with typical measured peak widths of 4 s,and generated peak capacities of 225 in 15 min.After the UPLC-oaTOF-MS analysis,principal component analysis(PCA) was used for group differentiation and marker selection.In the projection of positive mode,DM/DN patients and the controls were obviously divided into three groups.Furthermore,two potential markers were identified as phytosphingosine and sphinganine,respectively.Phytosphingosine and sphinganine with decreased concentrations in the patients,were closely related to the sphingolipid metabolism.
文摘目的建立骨刺胶囊（昆布、骨碎补、白芍、党参等）指纹图谱,并结合质谱信息鉴定特征峰的化学结构信息。方法骨刺胶囊75%甲醇提取液的分析采用Phenomenex Luna C18柱（4.6 mm×250 mm,5μm）;流动相为乙腈-20 mmol/L甲酸铵水溶液体系;体积流量为1.0 m L/min,梯度洗脱;检测波长为254 nm。采用飞行时间质谱（TOFMS）结合离子阱多级质谱（Ion-trap/MSn）,鉴定骨刺胶囊指纹图谱中特征峰的结构,正、负两种离子模式扫描。结果骨刺胶囊HPLC-MS指认21个共有峰,表征昆布、白芍、杜仲、党参、马钱子、鸡血藤、骨碎补、延胡索和桂枝等9味药材的特征成分。以绿原酸为参照物峰,12批样品的相似度在0.821~0.945之间。结论该方法显示,骨刺胶囊主要化学成分相似,质量较稳定。
