建立同时测量百草枯、单甲脒2种极性农药的液相色谱—串联质普测定方法,采用SCX和C_(18)(质量比为1:20)复合材料的Shiseido CAPCELL PAK CR色谱柱分离,最后采用高压液相色谱—串联质谱仪检测。对质谱条件及色谱条件进行优化处理,蔬菜样...建立同时测量百草枯、单甲脒2种极性农药的液相色谱—串联质普测定方法,采用SCX和C_(18)(质量比为1:20)复合材料的Shiseido CAPCELL PAK CR色谱柱分离,最后采用高压液相色谱—串联质谱仪检测。对质谱条件及色谱条件进行优化处理,蔬菜样品采用甲酸—乙腈溶液均质进行提取,三氯甲烷去除色素,并在定量限1、20、10倍浓度水平处理,其中百草枯回收率在61.8%~97.0%,单甲脒62.2%~100.0%,且测定结果的相对标准偏差≤5.61%。该方法简单快速,可用于蔬菜极性农药中百草枯、单甲脒等残留量的测定。展开更多
To establish a rapid and effective method for analysis and identification of the alkaloids from Ranunculus japoni- cus Thunb by ultra-performance liquid chromatogaraphy with quadruple-time-of-flight mass spectrometry ...To establish a rapid and effective method for analysis and identification of the alkaloids from Ranunculus japoni- cus Thunb by ultra-performance liquid chromatogaraphy with quadruple-time-of-flight mass spectrometry （UPLC/Q-TOF- MS） and discuss their fragmentation regularity, the UPLC/Q-TOF-MS was used to identify the alkaloids from Ranunculus japonicus Thunb by their MS data, tandem characteristic fragment ions and standards. In the end, 12 alkaloids were identi- fied from Ranunculus japonicus for the first time, and their fragmentation regularity was discussed. Thus, a rapid and effec- tive analysis and identification method for the alkaloids from Ranunculus japonicus by UPLC/Q-TOF-MS is established.展开更多
[Objective] This study aimed to develop a method of C_18-functionalized magnetic silica nanoparticles solid phase extraction-high performance liquid chro- matography-tandem mass spectrometry for the determination of s...[Objective] This study aimed to develop a method of C_18-functionalized magnetic silica nanoparticles solid phase extraction-high performance liquid chro- matography-tandem mass spectrometry for the determination of sulfadimidine in royal jelly. [Method] The royal jelly samples were pretreated by MCX SPE column and C_18-functionalized magnetic silica nanoparticles, and the purified samples were de- tected by HPLC-MS/MS. [Result] The detection method showed a good linear rela- tionship in the range of 5-80 ugkg （r=0.993 1）. The recovery ranges were between 93%- 104% with the relative standard deviations （RSD） below 11.3%. [Conclusion] Combined with automation equipment, the method is simple, fast, time-saving, and easy to real- ize the automation of sulfadimidine in the royal jelly samples before determination.展开更多
The composition of fatty acids in triacylglycerides （TAGs） and their position on the glycerol backbone de- termine the nutritional value of vegetable oil. In this study, gas chromatography and high-performance liqui...The composition of fatty acids in triacylglycerides （TAGs） and their position on the glycerol backbone de- termine the nutritional value of vegetable oil. In this study, gas chromatography and high-performance liquid chromatography-tandem mass spectrometry （HPLC-MS/MS） were used to analyze the compo- sition and distribution of fatty acids in TAGs of different rapeseed oils. Our results show the content of oleic acid in higb-oleic-acid rapeseed oil to be about 80%. In terms of the number of acyl carbon atoms （CN）, TAGs with CN52-54 were most abundant, with a maximum concentration at CN54 （80%）. The main type of TAG was oleic-oleic-oleic （OOO）, accounting for 71.75%, while oleic-oleic-linoleic （OOL） accounted for ？.56%, oleic-oleic-linolenic （OOLn） accounted for 4.81%, and stearic-oleic-oleic （SO0） accounted for 4.74%. Oleic acid in high-oleic-acid rapeseed oil was distributed in the following order of preference： sn-2 〉 sn-1/3. In high-erucic-acid rapeseed oil, however, oleic acid was enriched at the sn-1/3. These data show that the content of oleic acid can be as high as about 80% in high-oleic-acid material. This finding suggests that high-oleic-acid rapeseed oil has high nutritional value.展开更多
Among pharmaceuticals and personal care products released into the aquatic environment, antibiotics are of particular concern, because of their ubiquity and health effects. Although scientists have recently paid more ...Among pharmaceuticals and personal care products released into the aquatic environment, antibiotics are of particular concern, because of their ubiquity and health effects. Although scientists have recently paid more attention to the threat of antibiotics to coastal ecosystems, researchers have often focused on relatively few antibiotics, because of the absence of suitable analytical methods. We have therefore developed a method for the rapid detection of 36 antibiotic residues in coastal waters, including tetracyclines （TCs）, sulfanilamides （SAs）, and quinolones （QLs）. The method consists of solid-phase extraction （SPE） and liquid chromatography-tandem mass spectrometry （LC-MS/MS） analysis, using electrospray ionization （ESI） in positive mode. The SPE was performed with Oasis HLB and Oasis MCX cartridges. Chromatographic separation on a Cr8 column was achieved using a binary eluent containing methanol and water with 0.1% formic acid. Typical recoveries of the analytes ranged from 67.4% to 109.3% at a fortification level of 100 ng/L. The precision of the method, calculated as relative standard deviation （RSD）, was below 14.6% for all the compounds. The limits of detection （LODs） varied from 0.45 pg to 7.97 pg. The method was applied to detemaine the target analytes in coastal waters of the Yellow Sea in Liaoning, China. Among the tested antibiotics, 31 were found in coastal ＇waters, with their concentrations between the LOD and 212.5 ng/L. These data indicate that this method is valid for analysis of antibiotics in coastal waters. The study first reports such a large number of antibiotics along the Yellow Sea coast of Liaoning, and should facilitate future comprehensive evaluation of antibiotics in coastal ecosystems展开更多
[Objective] A quick extraction method of QuEChERS-HPLC-MS/MS was established to determine forechlorfenuron in fruits and vegetables. [Method] Fruits and vegetables were extracted with 0.1% acetic acid of acetonitrile ...[Objective] A quick extraction method of QuEChERS-HPLC-MS/MS was established to determine forechlorfenuron in fruits and vegetables. [Method] Fruits and vegetables were extracted with 0.1% acetic acid of acetonitrile solution and pu- rified by QuEChERS, and then forechlorfenuron residues were determined by HPLC- MS/MS. [Result] The limits of detection （LODs） and low determination limit （LOQ） for the forechlorfenuron was 1.0 vg/kg and 5.0 pg/kg in fruits and vegetables, re- spectively. Regression equations of these hormones had a good linear relationship （FF〉0.999） within 2.0-100.0 vg/L. The average recoveries of forechlorfenuron was in the range of 72.0-115. 0% with the coefficients of variation between 1.5% and 9.8% at the spiked levels of 10.0-500.0 μg/kg. [Conclusion] The method can be applied for the determination of the forechlorfenuron in fruits and vegetables.展开更多
为了准确测定原料和产品中的总大豆异黄酮含量,建立了通过碱水解法将不稳定形式的大豆异黄酮(含丙二酰基和乙酰基)转化为稳定形式(含葡萄糖苷和苷元)的液相色谱-三重串联四极杆液质联用仪(liquid chromatography-triple tandem quadrupo...为了准确测定原料和产品中的总大豆异黄酮含量,建立了通过碱水解法将不稳定形式的大豆异黄酮(含丙二酰基和乙酰基)转化为稳定形式(含葡萄糖苷和苷元)的液相色谱-三重串联四极杆液质联用仪(liquid chromatography-triple tandem quadrupole liquid mass spectrometer,LC-MS/MS)测定方法,并进行了验证。去酰基化后总大豆异黄酮由大豆苷、黄豆苷、染料木苷、大豆苷元、黄豆苷元、染料木素这六种化合物组成。它们的线性范围分别为0.1~4.1μg/mL、0.11~4.36μg/mL、0.12~4.84μg/mL、0.1~4μg/mL、0.11~4.58μg/mL、0.11~4.37μg/mL。大豆异黄酮原料和产品药片的相对标准偏差(RSD)分别为4%和2%,原料和片剂中各成分的回收率均在90%~110%之间,且所有组分分析完成时间不超过10分钟。大豆异黄酮量的准确测定保证了大豆异黄酮类原料中规定的异黄酮量,以及产品标签上的正确异黄酮量。展开更多
文摘建立同时测量百草枯、单甲脒2种极性农药的液相色谱—串联质普测定方法,采用SCX和C_(18)(质量比为1:20)复合材料的Shiseido CAPCELL PAK CR色谱柱分离,最后采用高压液相色谱—串联质谱仪检测。对质谱条件及色谱条件进行优化处理,蔬菜样品采用甲酸—乙腈溶液均质进行提取,三氯甲烷去除色素,并在定量限1、20、10倍浓度水平处理,其中百草枯回收率在61.8%~97.0%,单甲脒62.2%~100.0%,且测定结果的相对标准偏差≤5.61%。该方法简单快速,可用于蔬菜极性农药中百草枯、单甲脒等残留量的测定。
文摘To establish a rapid and effective method for analysis and identification of the alkaloids from Ranunculus japoni- cus Thunb by ultra-performance liquid chromatogaraphy with quadruple-time-of-flight mass spectrometry （UPLC/Q-TOF- MS） and discuss their fragmentation regularity, the UPLC/Q-TOF-MS was used to identify the alkaloids from Ranunculus japonicus Thunb by their MS data, tandem characteristic fragment ions and standards. In the end, 12 alkaloids were identi- fied from Ranunculus japonicus for the first time, and their fragmentation regularity was discussed. Thus, a rapid and effec- tive analysis and identification method for the alkaloids from Ranunculus japonicus by UPLC/Q-TOF-MS is established.
基金Supported by the Innovation Fund for Technology Based Firms of Ministry of Science and Technology(09C26214425280)the National Key Technology R&D Program during the 12th Five-Year Plan Period(2012BAK17B10)the International S&T Cooperation and Communication Program of China(2011DFA32930)~~
文摘[Objective] This study aimed to develop a method of C_18-functionalized magnetic silica nanoparticles solid phase extraction-high performance liquid chro- matography-tandem mass spectrometry for the determination of sulfadimidine in royal jelly. [Method] The royal jelly samples were pretreated by MCX SPE column and C_18-functionalized magnetic silica nanoparticles, and the purified samples were de- tected by HPLC-MS/MS. [Result] The detection method showed a good linear rela- tionship in the range of 5-80 ugkg （r=0.993 1）. The recovery ranges were between 93%- 104% with the relative standard deviations （RSD） below 11.3%. [Conclusion] Combined with automation equipment, the method is simple, fast, time-saving, and easy to real- ize the automation of sulfadimidine in the royal jelly samples before determination.
文摘The composition of fatty acids in triacylglycerides （TAGs） and their position on the glycerol backbone de- termine the nutritional value of vegetable oil. In this study, gas chromatography and high-performance liquid chromatography-tandem mass spectrometry （HPLC-MS/MS） were used to analyze the compo- sition and distribution of fatty acids in TAGs of different rapeseed oils. Our results show the content of oleic acid in higb-oleic-acid rapeseed oil to be about 80%. In terms of the number of acyl carbon atoms （CN）, TAGs with CN52-54 were most abundant, with a maximum concentration at CN54 （80%）. The main type of TAG was oleic-oleic-oleic （OOO）, accounting for 71.75%, while oleic-oleic-linoleic （OOL） accounted for ？.56%, oleic-oleic-linolenic （OOLn） accounted for 4.81%, and stearic-oleic-oleic （SO0） accounted for 4.74%. Oleic acid in high-oleic-acid rapeseed oil was distributed in the following order of preference： sn-2 〉 sn-1/3. In high-erucic-acid rapeseed oil, however, oleic acid was enriched at the sn-1/3. These data show that the content of oleic acid can be as high as about 80% in high-oleic-acid material. This finding suggests that high-oleic-acid rapeseed oil has high nutritional value.
基金Supported by Young Scientists Research Program (No. 2009507)the Key Laboratory of Marine Bioactive Substances and Modern Analytical Techniques (No. MBSMAT-2010-04),SOA of China
文摘Among pharmaceuticals and personal care products released into the aquatic environment, antibiotics are of particular concern, because of their ubiquity and health effects. Although scientists have recently paid more attention to the threat of antibiotics to coastal ecosystems, researchers have often focused on relatively few antibiotics, because of the absence of suitable analytical methods. We have therefore developed a method for the rapid detection of 36 antibiotic residues in coastal waters, including tetracyclines （TCs）, sulfanilamides （SAs）, and quinolones （QLs）. The method consists of solid-phase extraction （SPE） and liquid chromatography-tandem mass spectrometry （LC-MS/MS） analysis, using electrospray ionization （ESI） in positive mode. The SPE was performed with Oasis HLB and Oasis MCX cartridges. Chromatographic separation on a Cr8 column was achieved using a binary eluent containing methanol and water with 0.1% formic acid. Typical recoveries of the analytes ranged from 67.4% to 109.3% at a fortification level of 100 ng/L. The precision of the method, calculated as relative standard deviation （RSD）, was below 14.6% for all the compounds. The limits of detection （LODs） varied from 0.45 pg to 7.97 pg. The method was applied to detemaine the target analytes in coastal waters of the Yellow Sea in Liaoning, China. Among the tested antibiotics, 31 were found in coastal ＇waters, with their concentrations between the LOD and 212.5 ng/L. These data indicate that this method is valid for analysis of antibiotics in coastal waters. The study first reports such a large number of antibiotics along the Yellow Sea coast of Liaoning, and should facilitate future comprehensive evaluation of antibiotics in coastal ecosystems
文摘[Objective] A quick extraction method of QuEChERS-HPLC-MS/MS was established to determine forechlorfenuron in fruits and vegetables. [Method] Fruits and vegetables were extracted with 0.1% acetic acid of acetonitrile solution and pu- rified by QuEChERS, and then forechlorfenuron residues were determined by HPLC- MS/MS. [Result] The limits of detection （LODs） and low determination limit （LOQ） for the forechlorfenuron was 1.0 vg/kg and 5.0 pg/kg in fruits and vegetables, re- spectively. Regression equations of these hormones had a good linear relationship （FF〉0.999） within 2.0-100.0 vg/L. The average recoveries of forechlorfenuron was in the range of 72.0-115. 0% with the coefficients of variation between 1.5% and 9.8% at the spiked levels of 10.0-500.0 μg/kg. [Conclusion] The method can be applied for the determination of the forechlorfenuron in fruits and vegetables.
文摘为了准确测定原料和产品中的总大豆异黄酮含量,建立了通过碱水解法将不稳定形式的大豆异黄酮(含丙二酰基和乙酰基)转化为稳定形式(含葡萄糖苷和苷元)的液相色谱-三重串联四极杆液质联用仪(liquid chromatography-triple tandem quadrupole liquid mass spectrometer,LC-MS/MS)测定方法,并进行了验证。去酰基化后总大豆异黄酮由大豆苷、黄豆苷、染料木苷、大豆苷元、黄豆苷元、染料木素这六种化合物组成。它们的线性范围分别为0.1~4.1μg/mL、0.11~4.36μg/mL、0.12~4.84μg/mL、0.1~4μg/mL、0.11~4.58μg/mL、0.11~4.37μg/mL。大豆异黄酮原料和产品药片的相对标准偏差(RSD)分别为4%和2%,原料和片剂中各成分的回收率均在90%~110%之间,且所有组分分析完成时间不超过10分钟。大豆异黄酮量的准确测定保证了大豆异黄酮类原料中规定的异黄酮量,以及产品标签上的正确异黄酮量。
