[Method] This study aimed to determine trace amount of polycyclic aromatic hydrocarbons(PAHs) in urban sewage by using solid-phase extraction(SPE) coupled with high performance liquid chromatograph(HPLC).[Method] From...[Method] This study aimed to determine trace amount of polycyclic aromatic hydrocarbons(PAHs) in urban sewage by using solid-phase extraction(SPE) coupled with high performance liquid chromatograph(HPLC).[Method] From the aspects of solid-phase extraction column,elution solvent,elution volume,elution speed and so forth,the test conditions of SPE-HPLC method were optimized,and trace amount of PAHs in urban sewage was determined.[Result] The optimized solid-phase extraction conditions were SUPELCLEAN LC-18 solid-phase extraction column,methylene dichloride as elution solvent,15 ml elution volume,2 ml/min elution speed,5 ml/min loading speed,1 000 ml water with 200 ml methanol loading volume.Under the optimized extraction conditions,the recovery was high,namely 76.3%-105.2%;relative standard deviation was 3.8%-6.0%,showing good precision;detection limit was low,only 0.000 8-0.048 0 μg/L.[Conclusion] This method is user-friendly,with high sensitivity and good precision,and suitable for continuous determination of a large volume of water samples.展开更多
Dexamethasone is classified as a corticosteroid and is commonly used among cancer patients to decrease the amount of swelling around the tumor. Among patients with cancer, in particular brain tumors, seizures can beco...Dexamethasone is classified as a corticosteroid and is commonly used among cancer patients to decrease the amount of swelling around the tumor. Among patients with cancer, in particular brain tumors, seizures can become a daily routine in their everyday lives. To counteract the seizures, an antiepileptic drug such as phenytoin is administered to act as an anticonvulsant. Phenytoin and dexamethasone are frequently administrated concurrently to brain cancer patients. A previous study has shown that phenytoin serum concentration decreases when administrated concurrently with dexamethasone. Thus, it is important to monitor the concentration of these two drugs in biological samples to ensure that the proper dosages are administrated to the patients. This study aims to develop an effective extraction and detection method for dexamethasone and phenytoin. A reverse-phase high-performance liquid chromatography (HPLC) method with UV/Vis detection has been developed to separate phenytoin and dexamethasone at 219 nm and 241 nm respectively from urine samples. The mobile phase consists of a mixture of 0.01 M KH2PO4, acetonitrile, and methanol adjusted to pH 5.6 (48:32:20) and is pumped at a flow rate of 1.0 mL/min. Calibration curves were prepared for phenytoin and dexamethasone (r2 > 0.99). An efficient solid-phase extraction (SPE) method for the extraction of dexamethasone and phenytoin from urine samples was developed with the use of C-18 cartridges. The percent recovery for phenytoin and dexamethasone is 95.4% (RSD = 1.15%) and 81.1% (RSD = 3.56%) respectively.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
In this study,a hydrophilic resin named GCHM was fabricated based on poly(N-vinyl pyrrolidone-codivinylbenzene),characterized,and applied as a solid-phase extraction(SPE)material.Up to 44 pharmaceuticals and personal ...In this study,a hydrophilic resin named GCHM was fabricated based on poly(N-vinyl pyrrolidone-codivinylbenzene),characterized,and applied as a solid-phase extraction(SPE)material.Up to 44 pharmaceuticals and personal care products(PPCPs)belonging to 10 classes were recovered in environmental water samples.Different variables affecting extraction,such as adsorbent amount,sample pH,and loading speed,were optimized.Under optimal conditions,the average absolute recovgy of 44 PPCPs was 75.6%using GCHM,indicating a better performance than the commercial Oasis^HLB.SPE with home-made hydrophilic polymeric sorbent followed by ultra-performance liquid chromatography and tandem mass spectrometry was validated,and the method achieved good linearity(r2>0.991,for all analytes).In addition,the method detection limits of target compounds ranged from 0.03 to 0.6 ng/L.The developed method was applied to determine PPCPs in 10 environmental water samples taken from the Yangtze River,Huaihe River,and Taihu Lake,1 groundwater sample from Changzhou in Jiangsu Province,1 wastewater sample from Xiamen and 2 seawater samples from the Jiulong River in Fujian Province,China.In these samples,22 compounds were determined at levels ranging from 0.5 to 1590 ng/L.展开更多
Amantadine （AMA） is an anti-viral drug used in apiculture to protect honeybee against the sacbrood virus （Morator aetatulae）. This study described a reliable high-performance liquid chromatographic （HPLC） method...Amantadine （AMA） is an anti-viral drug used in apiculture to protect honeybee against the sacbrood virus （Morator aetatulae）. This study described a reliable high-performance liquid chromatographic （HPLC） method for analyzing AMA in honey using a solid-phase extraction （SPE） cartridge （Plexa PCX） for purification, 4-fluoro-7- nitro-2,1,3-benzoxadiazole （NBD-F） as a pre-column derivatization agent, and fluorometric detection （λex =470 nm, λem=530 nm）. The chromatographic separation was performed on an XDB C18 column （150×4.6 mm i.d.） using 0.1% trifluoroacetic acid/acetonitrile （35 ; 65, V/V） as the mobile phase at a flow rate of 1.0 mLomin 1 with a run time of 20 min. Under these optimal conditions, a linear relationship was observed in the range of 0.025--1.0μg·mL-1 with a good correlation coefficient （0.998） and low limit of detection （0.0080 μg·g-1）, the recoveries were all above 90%, and the intra-day and inter-day precision （RSD） ranged from 3.4%--5.1%.展开更多
基金Supported by National Science and Technology Key Project of Water Pollution Control and Management (2012ZX07209-003)
文摘[Method] This study aimed to determine trace amount of polycyclic aromatic hydrocarbons(PAHs) in urban sewage by using solid-phase extraction(SPE) coupled with high performance liquid chromatograph(HPLC).[Method] From the aspects of solid-phase extraction column,elution solvent,elution volume,elution speed and so forth,the test conditions of SPE-HPLC method were optimized,and trace amount of PAHs in urban sewage was determined.[Result] The optimized solid-phase extraction conditions were SUPELCLEAN LC-18 solid-phase extraction column,methylene dichloride as elution solvent,15 ml elution volume,2 ml/min elution speed,5 ml/min loading speed,1 000 ml water with 200 ml methanol loading volume.Under the optimized extraction conditions,the recovery was high,namely 76.3%-105.2%;relative standard deviation was 3.8%-6.0%,showing good precision;detection limit was low,only 0.000 8-0.048 0 μg/L.[Conclusion] This method is user-friendly,with high sensitivity and good precision,and suitable for continuous determination of a large volume of water samples.
文摘Dexamethasone is classified as a corticosteroid and is commonly used among cancer patients to decrease the amount of swelling around the tumor. Among patients with cancer, in particular brain tumors, seizures can become a daily routine in their everyday lives. To counteract the seizures, an antiepileptic drug such as phenytoin is administered to act as an anticonvulsant. Phenytoin and dexamethasone are frequently administrated concurrently to brain cancer patients. A previous study has shown that phenytoin serum concentration decreases when administrated concurrently with dexamethasone. Thus, it is important to monitor the concentration of these two drugs in biological samples to ensure that the proper dosages are administrated to the patients. This study aims to develop an effective extraction and detection method for dexamethasone and phenytoin. A reverse-phase high-performance liquid chromatography (HPLC) method with UV/Vis detection has been developed to separate phenytoin and dexamethasone at 219 nm and 241 nm respectively from urine samples. The mobile phase consists of a mixture of 0.01 M KH2PO4, acetonitrile, and methanol adjusted to pH 5.6 (48:32:20) and is pumped at a flow rate of 1.0 mL/min. Calibration curves were prepared for phenytoin and dexamethasone (r2 > 0.99). An efficient solid-phase extraction (SPE) method for the extraction of dexamethasone and phenytoin from urine samples was developed with the use of C-18 cartridges. The percent recovery for phenytoin and dexamethasone is 95.4% (RSD = 1.15%) and 81.1% (RSD = 3.56%) respectively.
基金Authors gratefully acknowledge the generous support provided by the National Key R&D Program of China(Grant No.2016YFE0112300)the National Natural Science Foundation of China(Grant Nos.51678290,51438008 and 51778281)+3 种基金Jiangsu Natural Science Fund,China(No.B K 20171342)Jiangsu Provincial Key Medical Discipline(Laboratory)of China(No.Z D X K A 2016008)Jiangsu Preventive Medicine Project of China(No.Y2018081)The authors also thank Dr.Zhe Wang from Nanyang Technological University(Singapore)for his support on this project.
文摘In this study,a hydrophilic resin named GCHM was fabricated based on poly(N-vinyl pyrrolidone-codivinylbenzene),characterized,and applied as a solid-phase extraction(SPE)material.Up to 44 pharmaceuticals and personal care products(PPCPs)belonging to 10 classes were recovered in environmental water samples.Different variables affecting extraction,such as adsorbent amount,sample pH,and loading speed,were optimized.Under optimal conditions,the average absolute recovgy of 44 PPCPs was 75.6%using GCHM,indicating a better performance than the commercial Oasis^HLB.SPE with home-made hydrophilic polymeric sorbent followed by ultra-performance liquid chromatography and tandem mass spectrometry was validated,and the method achieved good linearity(r2>0.991,for all analytes).In addition,the method detection limits of target compounds ranged from 0.03 to 0.6 ng/L.The developed method was applied to determine PPCPs in 10 environmental water samples taken from the Yangtze River,Huaihe River,and Taihu Lake,1 groundwater sample from Changzhou in Jiangsu Province,1 wastewater sample from Xiamen and 2 seawater samples from the Jiulong River in Fujian Province,China.In these samples,22 compounds were determined at levels ranging from 0.5 to 1590 ng/L.
文摘Amantadine （AMA） is an anti-viral drug used in apiculture to protect honeybee against the sacbrood virus （Morator aetatulae）. This study described a reliable high-performance liquid chromatographic （HPLC） method for analyzing AMA in honey using a solid-phase extraction （SPE） cartridge （Plexa PCX） for purification, 4-fluoro-7- nitro-2,1,3-benzoxadiazole （NBD-F） as a pre-column derivatization agent, and fluorometric detection （λex =470 nm, λem=530 nm）. The chromatographic separation was performed on an XDB C18 column （150×4.6 mm i.d.） using 0.1% trifluoroacetic acid/acetonitrile （35 ; 65, V/V） as the mobile phase at a flow rate of 1.0 mLomin 1 with a run time of 20 min. Under these optimal conditions, a linear relationship was observed in the range of 0.025--1.0μg·mL-1 with a good correlation coefficient （0.998） and low limit of detection （0.0080 μg·g-1）, the recoveries were all above 90%, and the intra-day and inter-day precision （RSD） ranged from 3.4%--5.1%.
