建立灵敏、可靠的中药材中农药多残留的检测方法对保证中药材的质量和安全十分重要。制备了磁性亲水亲脂平衡萃取材料Fe_(3)O_(4)@PLS,将其应用于农药多残留的磁性基质固相分散萃取中,并结合高效液相色谱-串联质谱法(HPLC-MS/MS)检测了...建立灵敏、可靠的中药材中农药多残留的检测方法对保证中药材的质量和安全十分重要。制备了磁性亲水亲脂平衡萃取材料Fe_(3)O_(4)@PLS,将其应用于农药多残留的磁性基质固相分散萃取中,并结合高效液相色谱-串联质谱法(HPLC-MS/MS)检测了金银花、菊花和三七块根(干)3种中药材中76种农药残留量。研究通过扫描电子显微镜(SEM)、傅里叶变换红外光谱(FT-IR)和X-射线衍射仪(XRD)对磁性萃取材料Fe_(3)O_(4)@PLS进行表面形貌和结构的表征。同时考察了影响磁性基质固相分散萃取效率的主要因素,结果表明,磁性萃取材料Fe_(3)O_(4)@PLS的用量为10 mg、研磨分散吸附时间为5 min、淋洗液为10 mL 20%(v/v)甲醇水溶液、涡旋振荡清洗1 min、以0.5 mL 0.1%(v/v)甲酸乙腈为洗脱剂、涡旋振荡洗脱1 min,76种农药的萃取效果最佳。在实际应用中,76种农药在金银花、菊花、三七块根(干)3种中药材中的萃取回收率别为69.1%~112.2%、67.1%~102.8%和70.1%~105.1%,相对标准偏差分别为2.0%~12.4%、2.1%~13.2%和2.0%~13.5%。该方法利用Fe_(3)O_(4)@PLS良好的磁响应性和亲水亲脂通用吸附特性,可以同时萃取极性农药(如多菌灵等)和非极性农药(如敌瘟磷等),建立了测定中药材中76种农药残留的磁性基质固相分散萃取-高效液相色谱-串联质谱联用的分析方法,具有低消耗、操作简便、灵敏度高等优点,适用于非液态中药材基质中多种类农药残留的检测。展开更多
目的设计一种取脂工具,取出不同直径轴状脂肪,再移植于裸鼠后研究其存活差异,为临床中小体积量脂肪移植提供更加便捷的方式。方法以1 m L注射器为模板,设计内径为4、6、8、10 mm的4种不锈钢取脂工具。于2014年5月~2015年4月行自体脂肪...目的设计一种取脂工具,取出不同直径轴状脂肪,再移植于裸鼠后研究其存活差异,为临床中小体积量脂肪移植提供更加便捷的方式。方法以1 m L注射器为模板,设计内径为4、6、8、10 mm的4种不锈钢取脂工具。于2014年5月~2015年4月行自体脂肪移植的12例患者中,分别采用以上4种内径取脂工具抽取腹部脂肪标本。取64只3~4周龄免疫缺陷裸鼠,随机分为A、B、C、D 4组,每组16只。以裸鼠背部皮下间隙为移植受区,分别移植用内径为4、6、8、10 mm取脂工具取出的0.5 m L脂肪组织。脂肪植入后,观察各组裸鼠存活情况以及脂肪植入部位的外观。植入脂肪术后1、2、4、8周,测量移植脂肪质量;每组随机处死4只裸鼠,取出受区剩余移植脂肪进行大体观察、组织学以及免疫组织化学染色观察,计数完整脂肪细胞以及毛细血管。结果新型手术工具可以轻松取出不同直径的轴状脂肪。脂肪植入裸鼠背部皮下腔隙后,随时间延长隆起样外观均趋于平坦,但C、D组隆起程度优于A、B组;解剖动物可见C、D组脂肪保持正常形态,并有血管长入。脂肪植入后即刻及1周时,4组脂肪质量比较差异无统计学意义(P>0.05);2、4、8周时,A组明显小于其他3组(P<0.05),B组小于C、D组(P<0.05),C、D组间差异无统计学意义(P<0.05)。组织学及免疫组织化学染色观察显示,随时间延长,与其余3组比较,D组脂肪细胞形态完整性较好,坏死区域小,血管密度高。除植入后1周各组间差异无统计学意义(P>0.05)外,其余各时间点,A组完整脂肪细胞明显少于其余3组(P<0.05),B组少于C、D组(P<0.05)。各时间点随取脂内径增大,毛细血管数呈增加趋势,组间比较差异均有统计学意义(P<0.05)。结论新型脂肪移植工具的手术操作简便,减少了对组织边缘的压迫。在10 mm范围内,取脂工具内径较大,可更好的保持组织完整性,脂肪植入裸鼠体内后血管密度更高、再血管化时间更短,形态维持的时间更持久。展开更多
Aim To develop and determine pinoresinol diglucopyranoside in Qing'e Pill, atraditional Chinese compound preparation containing Eucommia ulmoides Oliv. as the principal drug,by a reverse-phase high-performance liq...Aim To develop and determine pinoresinol diglucopyranoside in Qing'e Pill, atraditional Chinese compound preparation containing Eucommia ulmoides Oliv. as the principal drug,by a reverse-phase high-performance liquid chromatographic method (RP-HPLC) . Methods The extract ofQing'e Pill was refluxed with 75% ethanol, purified on an AB-8 macroporous adsorption resin columnand then injected into HPLC system. The HPLC assay was performed on an ODS analytical column with amixture of methanol-acetonitrile-water (24:3:78, V/V/V) as the mobile phase at a flow-rate of 1.0mL·min^(-1), and a UV detector set at 227 nm. Results Good linearity between peak area andconcentration was found in the range of 5.5 - 170 μg·mL^(-1) for pinoresinol diglucopyranoside ( r> 0.9998) . The average recovery was 99.3%. The intra-day assay RSD and the inter-day assay RSDwere 1.3% and 2.8%, respectively (n = 5). The content of pinoresinol diglucopyranoside in Qing'ePill was determined to be 0.446 +- 0.012 mg·g^(-1) (n = 10). Conclusion The RP-HPLC method wasproved to be sensitive, specific, accurate and precise for the determination of pinoresinoldiglucopyranoside in Qing' e Pill.展开更多
Ionic liquid (IL) trihexyl (tetradecyl) phosphonium bis 2,4,4-trimethylpentylphosphinate (Cyphos IL 104) was impregnated on XAD-7 resin. The solvent impreganated resin (SIR) was prepared and applied in Cr(VI) removal....Ionic liquid (IL) trihexyl (tetradecyl) phosphonium bis 2,4,4-trimethylpentylphosphinate (Cyphos IL 104) was impregnated on XAD-7 resin. The solvent impreganated resin (SIR) was prepared and applied in Cr(VI) removal. The morphology and the thermal stability of the resins were explored. The effects of equilibrium time and initial pH value on Cr(VI) adsorption were investigated. Adsorption isotherm, separation and desorption of the SIR, and selectivity of SIR were also explored. The results show that Cyphos IL 104 exists in the inner XAD-7 resin, and the optimum pH value range of the SIR for Cr(VI) extraction is 0 to 2. When NaOH used as desorption solution, the Cr(VI) can be effectively desorbed from the SIR.展开更多
建立超高效液相色谱-串联质谱测定全蛋粉中双酚A和双酚S的检测方法。全蛋粉经水复溶后经乙腈提取,提取液使用分散系固相萃取-基质增强脂质去除产品进行除脂,使用Oasis PRiME HLB小柱进一步净化,使用超高效液相串联质谱测定,负离子多反...建立超高效液相色谱-串联质谱测定全蛋粉中双酚A和双酚S的检测方法。全蛋粉经水复溶后经乙腈提取,提取液使用分散系固相萃取-基质增强脂质去除产品进行除脂,使用Oasis PRiME HLB小柱进一步净化,使用超高效液相串联质谱测定,负离子多反应监测(MRM)模式测定,内标法定量。结果显示:双酚A在1~50μg/kg范围内呈线性,相关系数为0.9991,加标回收率为98.8%~105.0%,日内和日间相对标准偏差分别为3.84%~8.58%和5.65%~8.74%,检出限为0.3μg/kg,定量限为1.0μg/kg;双酚S在0.4~20μg/kg范围内呈线性,相关系数为0.9995,加标回收率为98.5%~102.5%,日内和日间相对标准偏差分别为3.01%~7.86%和3.18%~7.03%,检出限为0.1μg/kg,定量限为0.3μg/kg。实际样品测定结果分别为:双酚A 2.4~3.8μg/kg;双酚S 0.48~0.82μg/kg。本方法前处理简单、高灵敏度适用于全蛋粉中双酚A和双酚S的日常测定。展开更多
A new method for simultaneous determination of four phthalate esters ( PAEs) in commercial fat-containing foods was developed by the combination of a packed nanofibers column based on solid-phase extraction with gas...A new method for simultaneous determination of four phthalate esters ( PAEs) in commercial fat-containing foods was developed by the combination of a packed nanofibers column based on solid-phase extraction with gas chromatography-flame ionization detector ( GC-FID ). Conditions for obtaining optimum extraction efficiency such as extraction solvents, morphologies of adsorbent, ion strength and pH were investigated and optimized in detail. Under the optimized conditions, the limits of detection (LODs) found for dibutyl phthalate (DBP) , butyl benzyl phthalate (BBP), diethyl hexyl phthalate (DEHP) and di-n-octyl phthalate (DNOP) were 50, 25, 50 and 25 ng/g, respectively. Good linearity of four PAEs was achieved in the range of 50 to 4 000 ng/g. The proposed method was applied for analyzing different kinds of fat-containing samples. PAEs in commercial fat-containing samples can be highly extracted by a packed solid-phase extraction column of 5 mg polystyrene ( PS) nanofibers. The satisfactory average recoveries were obtained in the range of 96. 7% to 102. 3% , and the relative standard deviations (RSDs) below 5% were achieved. The proposed method reduces the organic solvent consumption, the complex and tedious procedures for sample pretreatment, and achieves high sensitivity and reproducibility for the investigated PAEs.展开更多
To develop a simple and rapid purification method of rohitukine from the stem bark of Dysoxylum binectariferum. A L9 (34) orthogonal test was designed to optimize the extraction condition. Rohitukine in the plant e...To develop a simple and rapid purification method of rohitukine from the stem bark of Dysoxylum binectariferum. A L9 (34) orthogonal test was designed to optimize the extraction condition. Rohitukine in the plant extract was purified by using solvent-solvent partition and cation exchange resion (CER). Five different types of packing materials, including XAD-2 resin, polyamide, Sephadex LH-20, ODS and CER, were compared and CER showed the best capacity for rohitukine separation. The purification procedure was optimized as follows: the plant material powder was extracted with 70% ethanol (v/m = 60) by ultrasonic agitation for 60 min, then the 70% ethanol extract was dissolved in aqueous solution (pH 1, adjusted with 0.5 mol/L HCl) and extracted with equal volume of n-butanol. The aqueous layer was retained and the pH was adjusted to 10 with 25% aqueous ammonia and a solventsolvent partition was performed with equal volume of n-butanol. The obtained n-butanol extract was dissolved in aqueous solution (pH 1, adjusted with 0.5 mol/L HCl), and purified by a CER column eluting with H2O and 70% ethanol (pH 10, adjusted with 25% aqueous ammonia), successively. Rohitukine existed in 70% ethanol eluate, with a purity up to 53.3%. The method developed in this study provides a simple and rapid approach for the preparation of rohitukine from the stem bark ofD. binectariferum.展开更多
文摘建立灵敏、可靠的中药材中农药多残留的检测方法对保证中药材的质量和安全十分重要。制备了磁性亲水亲脂平衡萃取材料Fe_(3)O_(4)@PLS,将其应用于农药多残留的磁性基质固相分散萃取中,并结合高效液相色谱-串联质谱法(HPLC-MS/MS)检测了金银花、菊花和三七块根(干)3种中药材中76种农药残留量。研究通过扫描电子显微镜(SEM)、傅里叶变换红外光谱(FT-IR)和X-射线衍射仪(XRD)对磁性萃取材料Fe_(3)O_(4)@PLS进行表面形貌和结构的表征。同时考察了影响磁性基质固相分散萃取效率的主要因素,结果表明,磁性萃取材料Fe_(3)O_(4)@PLS的用量为10 mg、研磨分散吸附时间为5 min、淋洗液为10 mL 20%(v/v)甲醇水溶液、涡旋振荡清洗1 min、以0.5 mL 0.1%(v/v)甲酸乙腈为洗脱剂、涡旋振荡洗脱1 min,76种农药的萃取效果最佳。在实际应用中,76种农药在金银花、菊花、三七块根(干)3种中药材中的萃取回收率别为69.1%~112.2%、67.1%~102.8%和70.1%~105.1%,相对标准偏差分别为2.0%~12.4%、2.1%~13.2%和2.0%~13.5%。该方法利用Fe_(3)O_(4)@PLS良好的磁响应性和亲水亲脂通用吸附特性,可以同时萃取极性农药(如多菌灵等)和非极性农药(如敌瘟磷等),建立了测定中药材中76种农药残留的磁性基质固相分散萃取-高效液相色谱-串联质谱联用的分析方法,具有低消耗、操作简便、灵敏度高等优点,适用于非液态中药材基质中多种类农药残留的检测。
文摘目的设计一种取脂工具,取出不同直径轴状脂肪,再移植于裸鼠后研究其存活差异,为临床中小体积量脂肪移植提供更加便捷的方式。方法以1 m L注射器为模板,设计内径为4、6、8、10 mm的4种不锈钢取脂工具。于2014年5月~2015年4月行自体脂肪移植的12例患者中,分别采用以上4种内径取脂工具抽取腹部脂肪标本。取64只3~4周龄免疫缺陷裸鼠,随机分为A、B、C、D 4组,每组16只。以裸鼠背部皮下间隙为移植受区,分别移植用内径为4、6、8、10 mm取脂工具取出的0.5 m L脂肪组织。脂肪植入后,观察各组裸鼠存活情况以及脂肪植入部位的外观。植入脂肪术后1、2、4、8周,测量移植脂肪质量;每组随机处死4只裸鼠,取出受区剩余移植脂肪进行大体观察、组织学以及免疫组织化学染色观察,计数完整脂肪细胞以及毛细血管。结果新型手术工具可以轻松取出不同直径的轴状脂肪。脂肪植入裸鼠背部皮下腔隙后,随时间延长隆起样外观均趋于平坦,但C、D组隆起程度优于A、B组;解剖动物可见C、D组脂肪保持正常形态,并有血管长入。脂肪植入后即刻及1周时,4组脂肪质量比较差异无统计学意义(P>0.05);2、4、8周时,A组明显小于其他3组(P<0.05),B组小于C、D组(P<0.05),C、D组间差异无统计学意义(P<0.05)。组织学及免疫组织化学染色观察显示,随时间延长,与其余3组比较,D组脂肪细胞形态完整性较好,坏死区域小,血管密度高。除植入后1周各组间差异无统计学意义(P>0.05)外,其余各时间点,A组完整脂肪细胞明显少于其余3组(P<0.05),B组少于C、D组(P<0.05)。各时间点随取脂内径增大,毛细血管数呈增加趋势,组间比较差异均有统计学意义(P<0.05)。结论新型脂肪移植工具的手术操作简便,减少了对组织边缘的压迫。在10 mm范围内,取脂工具内径较大,可更好的保持组织完整性,脂肪植入裸鼠体内后血管密度更高、再血管化时间更短,形态维持的时间更持久。
文摘Aim To develop and determine pinoresinol diglucopyranoside in Qing'e Pill, atraditional Chinese compound preparation containing Eucommia ulmoides Oliv. as the principal drug,by a reverse-phase high-performance liquid chromatographic method (RP-HPLC) . Methods The extract ofQing'e Pill was refluxed with 75% ethanol, purified on an AB-8 macroporous adsorption resin columnand then injected into HPLC system. The HPLC assay was performed on an ODS analytical column with amixture of methanol-acetonitrile-water (24:3:78, V/V/V) as the mobile phase at a flow-rate of 1.0mL·min^(-1), and a UV detector set at 227 nm. Results Good linearity between peak area andconcentration was found in the range of 5.5 - 170 μg·mL^(-1) for pinoresinol diglucopyranoside ( r> 0.9998) . The average recovery was 99.3%. The intra-day assay RSD and the inter-day assay RSDwere 1.3% and 2.8%, respectively (n = 5). The content of pinoresinol diglucopyranoside in Qing'ePill was determined to be 0.446 +- 0.012 mg·g^(-1) (n = 10). Conclusion The RP-HPLC method wasproved to be sensitive, specific, accurate and precise for the determination of pinoresinoldiglucopyranoside in Qing' e Pill.
基金Project (51174184) sponsored by the National Natural Science Foundation of ChinaProject (2012CBA01202) supported by the National Basic Research Program of ChinaProject (KGZD-EW-201-1) supported by the Key Research Program of the Chinese Academy of Sciences
文摘Ionic liquid (IL) trihexyl (tetradecyl) phosphonium bis 2,4,4-trimethylpentylphosphinate (Cyphos IL 104) was impregnated on XAD-7 resin. The solvent impreganated resin (SIR) was prepared and applied in Cr(VI) removal. The morphology and the thermal stability of the resins were explored. The effects of equilibrium time and initial pH value on Cr(VI) adsorption were investigated. Adsorption isotherm, separation and desorption of the SIR, and selectivity of SIR were also explored. The results show that Cyphos IL 104 exists in the inner XAD-7 resin, and the optimum pH value range of the SIR for Cr(VI) extraction is 0 to 2. When NaOH used as desorption solution, the Cr(VI) can be effectively desorbed from the SIR.
文摘建立超高效液相色谱-串联质谱测定全蛋粉中双酚A和双酚S的检测方法。全蛋粉经水复溶后经乙腈提取,提取液使用分散系固相萃取-基质增强脂质去除产品进行除脂,使用Oasis PRiME HLB小柱进一步净化,使用超高效液相串联质谱测定,负离子多反应监测(MRM)模式测定,内标法定量。结果显示:双酚A在1~50μg/kg范围内呈线性,相关系数为0.9991,加标回收率为98.8%~105.0%,日内和日间相对标准偏差分别为3.84%~8.58%和5.65%~8.74%,检出限为0.3μg/kg,定量限为1.0μg/kg;双酚S在0.4~20μg/kg范围内呈线性,相关系数为0.9995,加标回收率为98.5%~102.5%,日内和日间相对标准偏差分别为3.01%~7.86%和3.18%~7.03%,检出限为0.1μg/kg,定量限为0.3μg/kg。实际样品测定结果分别为:双酚A 2.4~3.8μg/kg;双酚S 0.48~0.82μg/kg。本方法前处理简单、高灵敏度适用于全蛋粉中双酚A和双酚S的日常测定。
基金The National Basic Research Program of China(973Program)(No.2012CB933302)the National Instrumental Research Program(No.2014YQ06077303)+1 种基金the National Natural Science Foundation of China(No.81172720,21307086)Suzhou Science and Technology Department Foundation(No.ZXG201441)
文摘A new method for simultaneous determination of four phthalate esters ( PAEs) in commercial fat-containing foods was developed by the combination of a packed nanofibers column based on solid-phase extraction with gas chromatography-flame ionization detector ( GC-FID ). Conditions for obtaining optimum extraction efficiency such as extraction solvents, morphologies of adsorbent, ion strength and pH were investigated and optimized in detail. Under the optimized conditions, the limits of detection (LODs) found for dibutyl phthalate (DBP) , butyl benzyl phthalate (BBP), diethyl hexyl phthalate (DEHP) and di-n-octyl phthalate (DNOP) were 50, 25, 50 and 25 ng/g, respectively. Good linearity of four PAEs was achieved in the range of 50 to 4 000 ng/g. The proposed method was applied for analyzing different kinds of fat-containing samples. PAEs in commercial fat-containing samples can be highly extracted by a packed solid-phase extraction column of 5 mg polystyrene ( PS) nanofibers. The satisfactory average recoveries were obtained in the range of 96. 7% to 102. 3% , and the relative standard deviations (RSDs) below 5% were achieved. The proposed method reduces the organic solvent consumption, the complex and tedious procedures for sample pretreatment, and achieves high sensitivity and reproducibility for the investigated PAEs.
基金Scientific Research Foundation for the Returned Overseas Chinese Scholars by Ministry of Education of China (Grant No.[2004]527).
文摘To develop a simple and rapid purification method of rohitukine from the stem bark of Dysoxylum binectariferum. A L9 (34) orthogonal test was designed to optimize the extraction condition. Rohitukine in the plant extract was purified by using solvent-solvent partition and cation exchange resion (CER). Five different types of packing materials, including XAD-2 resin, polyamide, Sephadex LH-20, ODS and CER, were compared and CER showed the best capacity for rohitukine separation. The purification procedure was optimized as follows: the plant material powder was extracted with 70% ethanol (v/m = 60) by ultrasonic agitation for 60 min, then the 70% ethanol extract was dissolved in aqueous solution (pH 1, adjusted with 0.5 mol/L HCl) and extracted with equal volume of n-butanol. The aqueous layer was retained and the pH was adjusted to 10 with 25% aqueous ammonia and a solventsolvent partition was performed with equal volume of n-butanol. The obtained n-butanol extract was dissolved in aqueous solution (pH 1, adjusted with 0.5 mol/L HCl), and purified by a CER column eluting with H2O and 70% ethanol (pH 10, adjusted with 25% aqueous ammonia), successively. Rohitukine existed in 70% ethanol eluate, with a purity up to 53.3%. The method developed in this study provides a simple and rapid approach for the preparation of rohitukine from the stem bark ofD. binectariferum.