共查询到20条相似文献，搜索用时 250 毫秒
1.
《实验技术与管理》2019,(9)
建立B-烟酰胺单核苷酸的液相色谱-串联质谱快速测定方法。采用Shim-packVP-ODS(150L×2.0 mm,5μm)色谱柱进行色谱分离,流动相为甲醇与0.1%乙酸水溶液,梯度洗脱12 min,流速为0.3 mL/min,在质谱正离子模式下用多反应离子监测模式进行定量测定。在0.1425-228μg/L的质量浓度范围内线性良好(r=0.9998),回收率为86.6%～108%,RSD为3.4%;重现性好,RSD为2.22%;方法的定量限0.1425μg/L(S/N为10),检出限为0.07μg/L(S/N为5)。该方法灵敏度高、选择性好,适用于蔬菜、水果营养价值分析及药用价值开发研究中B-烟酰胺单核苷酸的快速测定。 相似文献
2.
《实验室研究与探索》2013,(10):266-269
建立了酒中8种邻苯二甲酸酯的超高效液相色谱-串联质谱联用仪检测方法。白酒、葡萄酒、黄酒等经前处理后,使用Waters ACQUITY UPLC仪和Waters Quattro Premier三级四极杆质谱仪,采用超高效液相苯基反相色谱柱分离,甲醇-水流动相流速0.2 mL/min,进样量2.0μL,电喷雾离子化串联质谱分析检测。该方法专一性强,检测耗时短,定量准确。检测酒中邻苯二甲酸酯的线性范围0.510.0mg/L,检出限0.05 mg/L,回收率86.4%10.0mg/L,检出限0.05 mg/L,回收率86.4%104.7%,相对标准偏差小于8.7%。 相似文献
3.
液相色谱-串联质谱法快速测定纺织品中6种致敏性分散染料 总被引：2，自引：0，他引：2
应用高效液相色谱-三重串联四级杆质谱技术,建立了纺织品中6种致敏性分散染料同时测定的快速分析方法。纺织品样品经甲醇提取后直接上样测定,前处理简便快捷,适合大批量样品分析。利用三重四级杆串联质谱的多重反应监测技术(MRM),可以减小基质干扰,降低检出限和增加定量准确性。该方法定量限10×10-9,线性范围0.1～100μg/mL,添加回收率不低于90%,RSD5%。 相似文献
4.
建立一种用于分析正山小种红茶中茶黄素的液相色谱-串联质谱法,利用多重反应监测模式对正山小种红茶中茶黄素进行定性和定量分析.色谱柱为反相C18柱,流动相为0.1%甲酸和乙腈,柱温35℃.分析结果表明:方法检出限为6.6 ng/g,相对标准偏差小于4.08%,回收率为91.2%～102.5%,该方法简便、快速、准确,适用于红茶中茶黄素的分析. 相似文献
5.
分析松针中16种有机磷农药和15种有机氯农药的残留量.通过对提取方法的比较,分析检测方法的优点与验证效果.在实验中,样品先经乙腈提取,再进行QuEChERS方法前处理,然后在多反应离子监测(MRM)模式下,通过气相色谱-串联质谱法(GC-MS/MS)对样品进行检测分析和外标法定量.结果表明：在该条件下,各种农药线性关系良好,线性相关系数大于0.98,精密度良好,RSD值在8.71%以内;当样品加标含量为2～10μg/L时,各种农药的平均回收率在68.48%～181.3%之间,RSD值在49.78%以下,方法的检测限低于0.005 mg/kg.该实验方法灵敏度高、准确性好,适用于林业多种有机磷和有机氯农药的残留检测. 相似文献
6.
建立了一种同时测定黄酒中亚砷酸根、砷酸根、砷甜菜碱、一甲基砷酸和二甲基砷酸等5种砷形态的高效液相色谱-电感耦合等离子体质谱(HPLC-ICP-MS)分析方法。黄酒经炭黑氨基柱净化,体积分数为10%甲醇水溶液洗脱,采用Hamilton PRP-XIO0阴离子交换色谱柱(4.1 mm×250 mm,10μm),60 mmol/L硝酸铵梯度洗脱,高效液相色谱分离,电感耦合等离子体质谱进行定性和定量分析。在0.5~20.0μg/L范围内各砷形态线性良好,相关系数R均>0.999;加标回收率85%~92%,相对标准偏差(RSD)1.4%~5.2%;5种砷形态的定量限均为0.10μg/L,检出限均为0.03μg/L。利用该方法对不同年份、不同企业及不同类型的黄酒进行了检测,该方法适用于黄酒中砷残留的分析检测。 相似文献
7.
建立了动物源性食品中9种喹诺酮类药物残留量的液相色谱-电喷雾串联四极杆质谱测定方法.样品经阳离子交换固相萃取柱净化后,采用多反应监测(MRM)模式,进行LC-MS/MS分析.方法检出限均为0.05μg/kg,在0.05～50μg/kg添加水平范围内,喹诺酮类药物回收率为65.8%～94.6%,相对标准偏差为5.3%～9.1%. 相似文献
8.
《河南职业技术师范学院学报(职业教育版)》2018,(6)
使用C8色谱柱,以体积分数为90%的甲醇水溶液为流动相,等度洗脱,多反应离子检测模式,监测离子对为m/z547.7→m/z305.4,建立了一次性使用输液器中偏苯三酸三辛酯(TOTM)溶出量的液相色谱-三重四极杆质谱联用(LC-MS/MS)检测方法.结果表明:TOTM质量浓度为5～150 ng/mL时,线性关系良好(r=0.999 4),检出限为0.5 ng/mL,相对标准偏差均小于2.27%,回收率在98.40%～100.22%之间.该方法操作简便、灵敏、准确、重现性好,适用于一次性使用输液器中TOTM的溶出量分析. 相似文献
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10.
食品或饲料中三聚氰胺和三聚氰酸经乙腈水萃取、提纯后,采用高效液相色谱(HPLC)法测定,外标法定量.对色谱分离条件进行了优化,三聚氰胺在0.1156～11.56 mg/L范围内线性良好,复相关系数r2=0.9997,平均加标回收率在95.59％～105.97％之间,相对标准偏差为0.14％～0.29％,检出限(S/N=3)为0.012 mg/L.三聚氰酸0.1020～10.20mg/L范围内线性良好,复相关系数为r2=0.9995,平均加标回收率在77.44％～88.77％之间,相对标准偏差为0.32％～0.86％,检出限(S/N=3)为0.051 mg/L.该法能满足食品或饲料中三聚氰胺和三聚氰酸检验工作的需要. 相似文献
11.
Huan-huan Pang Mei-fang Jiang Qin-hui Wang Xiao-ye Wang Wei Gao Zhi-hao Tian Jian-mei Huang 《Journal of Zhejiang University. Science. B》2018,19(3):227-244
Danshen, the dried root of Salvia miltiorrhiza Bunge (Lamiaceae), is one of the traditional Chinese medicines (TCMs) most commonly used for the treatment of cardiovascular and cerebrovascular diseases. However, little is known about the chemical and metabolic profiles of danshen in vitro or in vivo. In particular, more information is needed in relation to the 50% ethanol extracts usually used in danshen formulations such as Fufang Xueshuantong Capsules and Fufang Danshen tablets. High-performance liquid chromatography coupled with a linear ion trap- Orbitrap mass spectrometer (HPLC-LTQ-Orbitrap) provides a sensitive and accurate method for analyzing the composition of samples. This method was used to determine the in vitro and in vivo chemical and metabolic profiles of danshen. Sixty-nine components of danshen extract and 118 components of danshen in rat plasma, urine, feces, and bile were unambiguously or tentatively identified. These results not only revealed the material composition of danshen, but also provided a comprehensive research approach for the identification of multi-constituents in TCMs. 相似文献
12.
随着后基因组时代的到来,蛋白质组学研究的重要性日益显现出来。对于蛋白质结构、功能关系的研究由于局限于技术和手段的发展而进展缓慢。本文对将氢氘交换质谱联用的方法应用于研究蛋白质结构和功能之间关系的进展进行了综述,以期对初涉该领域的研究者以提示。 相似文献
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14.
佟健 《鞍山师范学院学报》2016,(2):48-51
采用电感耦合等离子体质谱法测定小麦中铅、砷、铬、镉、铜、锌、铁和锰8种重金属元素.用微波消解法对样品进行消解,用ICP-MS对消解液进行检测.用加标回收率试验考察了方法的准确性,结果表明,所测元素在标准溶液浓度范围内呈线性关系,相关系数均大于0.9990.方法的检出限在0.01025~4.547 mg/kg之间,相对标准偏差均小于3.89%,加标回收率在90.70%~109.9%之间.此方法快速准确、检出限低、灵敏度高,适用于小麦中8种重金属元素的测定. 相似文献
15.
Jiang JQ Zhang L Li GL Zhang HT Yang XF Liu JW Li RF Wang ZL Wang JH 《Journal of Zhejiang University. Science. B》2011,12(6):460-467
A rapid sample treatment procedure for the gas chromatography-tandem mass spectrometry (GC-MS) determination of 19-nortestosterone
(19-NT) in animal tissues has been developed. In our optimized procedures, enzymatic hydrolysis with β-glucuronidase from
Escherichia coli was performed in an acetate buffer (pH 5.2, 0.2 mol/L). Next, the homogenate was mixed with methanol and heated at 60 °C
for 15 min, then placed in an ice-bath at −18 °C for 2 h. After liquid-liquid extraction with n-hexane, the analytes were subjected to a normal-phase solid phase extraction (SPE) C18 cartridge for clean-up. The dried organic extracts were derivatized with heptafluorobutyric anhydride (HFBA), and then the
products were injected into GC-MS. Using electron impact mass spectrometry (EI-MS) with positive chemical ionization (PCI),
four diagnostic ions (m/z 666, 453, 318, and 306) were determined. A standard calibration curve over the concentration range of 1–20 ng/g was reached,
with Y=467 084X-68 354 (R
2=0.999 7) for 19-NT, and the detection limit was 0.3 ng. When applied to spiked samples collected from bovine and ovine, the
recoveries ranged from 63% to 101% with relative standard deviation (RSD) between 2.7% and 8.9%. The procedure is a highly
efficient, sensitive, and more economical method which offers considerable potential to resolve cases of suspected nandrolone
doping in husbandry animals. 相似文献
16.
《实验技术与管理》2015,(1)
建立了气相色谱-质谱联用(GC-MS)技术同时分析沉积物中三氯生和甲基三氯生的方法。采用丙酮提取沉积物样品,提取物经自制C18固相萃取柱净化,利用N-甲基-N(三甲基硅)-三氟乙酰胺(MSTFA)对提取物中三氯生进行衍生化,用外标法进行定量。GC-MS对三氯生和甲基三氯生的检出限分别为0.59ng/g和0.28ng/g,沉积物中三氯生和甲基三氯生不同浓度的加标回收率分别为85.6%~95.7%和84.4%~106.7%,相对标准偏差(RSD)分别为3.5%~6.9%和3.9%~6.3%。对6个沉积物样品进行了分析测定,三氯生和甲基三氯生的浓度分别为12.41~93.77ng/g和4.96~6.48ng/g。研究结果表明,该方法适用于同时测定沉积物样品中三氯生和甲基三氯生的含量,具有检出限低、灵敏度高、重复性好等优点,是一个较为可靠的检测方法。 相似文献
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采用微波消解法处理样品,利用电感耦合等离子体质谱法( ICP-MS)对大马哈鱼籽中的18种矿物元素进行分析测定.对样品的消化方法进行了考查,优化了仪器的工作参数.结果表明,所测元素校准方程的相关系数均大于0.9990,回收率范围为90.1%~108.1%,相对标准偏差为1.54%~7.57%.该方法简便、快速、准确、灵敏度高,可用于海产品中18种矿物元素的同时测定. 相似文献
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Xiao YP Wu TX Hong QH Sun JM Chen AG Yang CM Li XY 《Journal of Zhejiang University. Science. B》2012,13(7):567-578
A novel metabolomic method based on gas chromatography/mass spectrometry (GC-MS) was applied to determine the metabolites in the serum of piglets in response to weaning and dietary L-glutamine (Gln) supplementation. Thirty-six 21-d-old piglets were randomly assigned into three groups. One group continued to suckle from the sows (suckling group), whereas the other two groups were weaned and their diets were supplemented with 1% (w/w) Gln or isonitrogenous L-alanine, respectively, representing Gln group or control group. Serum samples were collected to characterize metabolites after a 7-d treatment. Results showed that twenty metabolites were down-regulated significantly (P<0.05) in control piglets compared with suckling ones. These data demonstrated that early weaning causes a wide range of metabolic changes across arginine and proline metabolism, aminosugar and nucleotide metabolism, galactose metabolism, glycerophospholipid metabolism, biosynthesis of unsaturated fatty acid, and fatty acid metabolism. Dietary Gln supplementation increased the levels of creatinine, D-xylose, 2-hydroxybutyric acid, palmitelaidic acid, and α-L-galactofuranose (P<0.05) in early weaned piglets, and were involved in the arginine and proline metabolism, carbohydrate metabolism, and fatty acid metabolism. A leave-one-out cross-validation of random forest analysis indicated that creatinine was the most important metabolite among the three groups. Notably, the concentration of creatinine in control piglets was decreased (P=0.00001) compared to the suckling piglets, and increased (P=0.0003) in Gln-supplemented piglets. A correlation network for weaned and suckling piglets revealed that early weaning changed the metabolic pathways, leading to the abnormality of carbohydrate metabolism, amino acid metabolism, and lipid metabolism, which could be partially improved by dietary Gln supplementation. These findings provide fresh insight into the complex metabolic changes in response to early weaning and dietary Gln supplementation in piglets. 相似文献
19.
建立固相萃取与UPLC—MS／MS检测食品中黄曲霉毒素M1和黄曲霉毒素B1的方法。样品经乙腈提取和SPE小柱萃取净化,提取液经氮气吹干后,用50％甲醇水溶液定容。超高效液相色谱一串联质谱（UPLC—MS／MS）测定,采用电喷雾正离子（ESI＋）模式电离,多反应监测（MRM）模式检测。流动相为0．1％甲酸水溶液和甲醇,流速0．4ml／min,使用ZORBAX Eclipse XDB—C18色谱柱（100mm×3．0mm×1．8μm）为分析柱。黄曲霉毒素AFM1在0．1～50μg／kg范围内线性关系良好、黄曲霉毒素AFB1在0．1～10ug／kg范围内线性关系良好,相关系数均大于0．999;回收率在83．75％～97．8％之间;检出限AFMl为0．05μg／kg、AFBl0．02μg／kg。该法具有分析速度快,检测准确、灵敏度和回收率高等优点,适合食品中黄曲霉毒素M1、B1含量的检测。 相似文献
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