建立一种固相萃取-高效液相色谱-串联质谱(Solid phase extraction coupled to high performance liquid chromatography tandem mass spectrometry,SPE-HPLC-MS/MS)检测动物源性食品中金刚烷胺残留的方法。研究采用Oasis MCX固相萃取...建立一种固相萃取-高效液相色谱-串联质谱(Solid phase extraction coupled to high performance liquid chromatography tandem mass spectrometry,SPE-HPLC-MS/MS)检测动物源性食品中金刚烷胺残留的方法。研究采用Oasis MCX固相萃取小柱为基质净化柱,以Agilent SB-C18柱(2.1 mm×150 mm,3.5μm)为液相分离柱,0.1%甲酸-乙腈为(体积比,80∶20)为流动相,流速0.2 m L/min。用电喷雾离子源正离子多反应监测(Multi-reaction monitoring,MRM)模式进行检测,外标法定量。在0.1μg/L^100.0μg/L范围内具有较好的线性关系,相关系数>0.999。该方法检出限(Limit of detection,LOD)为1.0μg/kg,定量限(Limit of quantitation,LOQ)为3.0μg/kg,对3个添加浓度(30.0、60.0、90.0μg/kg)下的鸡胸,鸡肝,鸡蛋,猪肉,羊肉5种样品中金刚烷胺残留的检测具有较高的准确度(回收率在83.6%~94.2%之间)和重现性(RSD<4.0%,n=3)。展开更多
A molecular imprinting polymer technique was successfully applied to precipitation polymerization by using styrene as a functional monomer, curcuminoids as templates, acetonitrile as a porogenic solvent,benzoyl peroxi...A molecular imprinting polymer technique was successfully applied to precipitation polymerization by using styrene as a functional monomer, curcuminoids as templates, acetonitrile as a porogenic solvent,benzoyl peroxide as the initiator, and ethylene glycol dimethacrylate as the crosslinker. The effects of interaction on the adsorption capacity of the molecularly imprinted polymer(MIP) and non-imprinted polymer(NIP) were investigated. A comparison of the adsorption capacity for MIP and NIP indicated that the NIP had the lowest adsorption capacity. The curcuminoid-imprinted polymer(Cur-MIP) was synthesized from 0.0237 mmol of styrene, 47.0 g of acetonitrile, 1.0238 mmol of ethylene glycol dimethacrylate, 0.0325 mmol of curcuminoids, and 0.2480 mmol of benzoyl peroxide. A high-performance liquid chromatography method with fluorescence detection was developed and validated for various chromatographic conditions for the determination of the curcuminoids in turmeric samples. The sample solution was separated using the Cur-MIP via solid-phase extraction and analyzed on a Brownlee analytical C_(18) column(150 mm ×6 mm, 5 mm) using an isocratic elution consisting of acetonitrile and 0.1%trichloroacetic acid(40:60, v/v). The flow rate was maintained at 1.5 m L/min. The fluorescence detector was set to monitor at λex? 426 nm and λem? 539 nm. The quantification limit values were found to be16.66, 66.66, and 33.33 mg/L for curcumin, demethoxycurcumin, and bisdemethoxycurcumin, respectively. Thus, we concluded that the Cur-MIP and high-performance liquid chromatographic-fluorescence method could be applied to selective extraction and could be used as a rapid tool for the determination of curcuminoids in medicinal herbal extracts.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
目的:建立吸毒人员血浆中儿茶酚胺及其代谢产物的高效液相色谱测定方法。方法:采用固相萃取方法对血浆样品进行预处理,利用高效液相色谱分离待测物,最后使用荧光检测器检测儿茶酚胺及其代谢产物。结果:以弱酸性乙酸盐缓冲体系/庚烷磺酸...目的:建立吸毒人员血浆中儿茶酚胺及其代谢产物的高效液相色谱测定方法。方法:采用固相萃取方法对血浆样品进行预处理,利用高效液相色谱分离待测物,最后使用荧光检测器检测儿茶酚胺及其代谢产物。结果:以弱酸性乙酸盐缓冲体系/庚烷磺酸钠离子对试剂/甲醇作为流动相,采用梯度洗脱的方式,7种儿茶酚胺及其代谢产物能完全分离。利用SUPELCO RIDA C18小柱处理加标血浆样品,在优化的最佳洗脱条件下,加标回收率在85.6%～106.3%范围内。方法的相对标准差(RSD)为2.3%～6.7%。各被测物质线性关系良好,相关系数均大于0.997,检出限为5.0μg/L～50.0μg/L。结论:该方法简便快速、灵敏度高,适用于血浆中儿茶酚胺及其代谢产物的测定。展开更多
文摘建立一种固相萃取-高效液相色谱-串联质谱(Solid phase extraction coupled to high performance liquid chromatography tandem mass spectrometry,SPE-HPLC-MS/MS)检测动物源性食品中金刚烷胺残留的方法。研究采用Oasis MCX固相萃取小柱为基质净化柱,以Agilent SB-C18柱(2.1 mm×150 mm,3.5μm)为液相分离柱,0.1%甲酸-乙腈为(体积比,80∶20)为流动相,流速0.2 m L/min。用电喷雾离子源正离子多反应监测(Multi-reaction monitoring,MRM)模式进行检测,外标法定量。在0.1μg/L^100.0μg/L范围内具有较好的线性关系,相关系数>0.999。该方法检出限(Limit of detection,LOD)为1.0μg/kg,定量限(Limit of quantitation,LOQ)为3.0μg/kg,对3个添加浓度(30.0、60.0、90.0μg/kg)下的鸡胸,鸡肝,鸡蛋,猪肉,羊肉5种样品中金刚烷胺残留的检测具有较高的准确度(回收率在83.6%~94.2%之间)和重现性(RSD<4.0%,n=3)。
文摘A molecular imprinting polymer technique was successfully applied to precipitation polymerization by using styrene as a functional monomer, curcuminoids as templates, acetonitrile as a porogenic solvent,benzoyl peroxide as the initiator, and ethylene glycol dimethacrylate as the crosslinker. The effects of interaction on the adsorption capacity of the molecularly imprinted polymer(MIP) and non-imprinted polymer(NIP) were investigated. A comparison of the adsorption capacity for MIP and NIP indicated that the NIP had the lowest adsorption capacity. The curcuminoid-imprinted polymer(Cur-MIP) was synthesized from 0.0237 mmol of styrene, 47.0 g of acetonitrile, 1.0238 mmol of ethylene glycol dimethacrylate, 0.0325 mmol of curcuminoids, and 0.2480 mmol of benzoyl peroxide. A high-performance liquid chromatography method with fluorescence detection was developed and validated for various chromatographic conditions for the determination of the curcuminoids in turmeric samples. The sample solution was separated using the Cur-MIP via solid-phase extraction and analyzed on a Brownlee analytical C_(18) column(150 mm ×6 mm, 5 mm) using an isocratic elution consisting of acetonitrile and 0.1%trichloroacetic acid(40:60, v/v). The flow rate was maintained at 1.5 m L/min. The fluorescence detector was set to monitor at λex? 426 nm and λem? 539 nm. The quantification limit values were found to be16.66, 66.66, and 33.33 mg/L for curcumin, demethoxycurcumin, and bisdemethoxycurcumin, respectively. Thus, we concluded that the Cur-MIP and high-performance liquid chromatographic-fluorescence method could be applied to selective extraction and could be used as a rapid tool for the determination of curcuminoids in medicinal herbal extracts.
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%.
文摘目的:建立吸毒人员血浆中儿茶酚胺及其代谢产物的高效液相色谱测定方法。方法:采用固相萃取方法对血浆样品进行预处理,利用高效液相色谱分离待测物,最后使用荧光检测器检测儿茶酚胺及其代谢产物。结果:以弱酸性乙酸盐缓冲体系/庚烷磺酸钠离子对试剂/甲醇作为流动相,采用梯度洗脱的方式,7种儿茶酚胺及其代谢产物能完全分离。利用SUPELCO RIDA C18小柱处理加标血浆样品,在优化的最佳洗脱条件下,加标回收率在85.6%～106.3%范围内。方法的相对标准差(RSD)为2.3%～6.7%。各被测物质线性关系良好,相关系数均大于0.997,检出限为5.0μg/L～50.0μg/L。结论:该方法简便快速、灵敏度高,适用于血浆中儿茶酚胺及其代谢产物的测定。
文摘建立固相萃取-高效液相色谱对小麦中脱氧雪腐镰刀菌烯醇（deoxynivalenol,DON）进行测定的方法。从提取溶剂、净化方式、流动相组成以及流动相流速等条件优化DON检测方法。结果表明,当样品提取溶剂为乙腈-水（84∶16,V/V）,Bond Elut Mycotoxin固相萃取柱净化,流动相组成为乙腈-水（6∶94,V/V）,流速为0.9 m L/min时,DON检测结果最好,该检测方法的DON回收率达到90.12%～106.25%,日内和日间相对标准偏差分别为4.51%和6.12%。该方法快速、准确,重复性好,稳定性高,适合DON污染小麦样品的大批量检测。
文摘建立了高效液相色谱-荧光检测(HPLC-FLD)测定橄榄油中苯并[a]蒽、屈艹、苯并[b]荧蒽、苯并[a]芘4种多环芳烃(PAHs)的分析方法。橄榄油样品经异丙醇稀释,采用具有π-π特异性作用的固相萃取柱净化,Agilent ZORBAX Eclipse PAH色谱柱(100 m m×2.1 m m,1.8μm)分离,以水-乙腈为流动相,梯度洗脱,实现了4种化合物的基线分离,并用基质匹配校准溶液进行外标法定量。4种多环芳烃的线性范围为2.4~40μg/L,相关系数(r)为0.999 0~0.999 9,方法的定量限为0.147~0.413μg/L,加标回收率为95.5%~103.2%,日内和日间精密度(RSD)分别为0.10%~1.69%和2.48%~2.93%(n=5)。该法具有灵敏度高、检出限低、重复性好等特点,适用于橄榄油中4种PAHs快速、准确的定量检测。
