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Simultaneous Determination of 14 β-Receptor Agonists Residues in Mutton by High Performance Liquid Chromatography-Tandem Mass Spectrometry (HPLC-MS/MS)
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作者 Zhe MENG Jianhua WANG +5 位作者 Bo LIU Yuhang GUO Haoshuang DONG Pingyang SHAN Dawei WANG Yajuan SONG 《Agricultural Biotechnology》 CAS 2023年第5期55-58,共4页
[Objectives]A high performance liquid chromatography-tandem mass spectrometry(HPLC-MS/MS)method was established for the determination of 14β-receptor agonist residues in mutton.[Methods]Samples were hydrolyzed byβ-g... [Objectives]A high performance liquid chromatography-tandem mass spectrometry(HPLC-MS/MS)method was established for the determination of 14β-receptor agonist residues in mutton.[Methods]Samples were hydrolyzed byβ-glucuronidase and extracted with 5%acetic acid-acetonitrile(1:99,V/V)solution.An Eclipse plus C 18 column was used for separation,and the MRM mode was used for qualitative analysis,and the external standard method was used for quantitative analysis of matrix standard solutions.[Results]Under the optimal conditions,the retention time of the 14 kinds ofβ-receptor agonists ranged from 1.0 to 9.5 min.When the mass concentration was in the range of 0.05-0.50μg/ml,the linear relationship ofβ-receptor agonists was good,with correlation coefficients(r)≥0.9992.The detection limits of the method were in the range of 0.04-0.87μg/kg,and the quantitative limits were in the range of 0.35-1.86μg/kg.The average recovery values were in the range of 82.8%-108.9%,with RSDs(n=6)in the range of 1.9%-6.7%.[Conclusions]The method is simple,sensitive,reproducible,accurate,and can be used for simultaneous determination of the 14 kinds ofβ-receptor agonist residues in mutton. 展开更多
关键词 MUTTON high performance liquid chromatography-tandem mass spectrometry β-receptor agonist RESIDUE
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Detection of 36 antibiotics in coastal waters using high performance liquid chromatography-tandem mass spectrometry 被引量:13
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作者 那广水 顾佳 +4 位作者 葛林科 张蓬 王震 刘春阳 张琳 《Chinese Journal of Oceanology and Limnology》 SCIE CAS CSCD 2011年第5期1093-1102,共10页
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
关键词 ANTIBIOTICS high performance liquid chromatography-tandem mass spectrometry SOLID-PHASEEXTRACTION coastal waters
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Determination of okadaic acid related toxins from shellfish (<i>sinonovacula constricta</i>) by high performance liquid chromatography tandem mass spectrometry
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作者 Hai-qi Zhang Weicheng Liu +3 位作者 Xin He Li-jun Liang Wenyong Ding Zhong-yang He 《Agricultural Sciences》 2013年第5期1-6,共6页
Consumption of shellfish contaminated with algal toxins produced by marine dinoflagellates can lead to diarrhetic shellfish poisoning (DSP). It was therefore essential that there are analytical techniques to identify ... Consumption of shellfish contaminated with algal toxins produced by marine dinoflagellates can lead to diarrhetic shellfish poisoning (DSP). It was therefore essential that there are analytical techniques to identify and quantify DSP toxins in shellfish. This new methodology could facilitate DSP monitoring and create a means of rapidly responding to incidents threatening public health. In the last years there were different analytical methods for DSP, such as mouse bioassay and LC-FLD. With the development of instrument, Liquid chromatography-mass spectrometry was substituted for other analytical methods with its good sensitivity and selectivity and without derivatization for the determination of DSP. In this report, a high performance liquid chromatogra-phytandem mass spectrometric(HPLC-MS/MS)method was developed for the simultaneous determination of okadaic acid (OA) and dinophysistoxins(DTX1) in Sinonovacula constricta. Optimization of pretreatment experiment was carried out to maximize recoveries and the effectiveness. The analytes were determined under multi-reactions monitoring (MRM) scan type with tandem mass analyzer using negative ion electrospray ionization (-ESI) mode .Finally, the detection and identification of OA and DTX-1 were based upon their retention times (RT) and the fragmentation patterns of their mass spectra. The method of LOQ for the two poisons was 0.02 mg·kg-1.The real sample test showed that this method could be used for sensitive, fast, and accurate determination of the two diarrheic shellfish poisons in shellfish. 展开更多
关键词 Sinonovacula Constricta high performance liquid chromatography-tandem mass spectrometry Okadaic Acid Dinophysistoxins-1
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Determination of chlorpromazine in porcine muscle using high performance liquid chromatography-tandem mass spectrometry
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作者 张露 黄雯 蒋心惠 《Journal of Chinese Pharmaceutical Sciences》 CAS CSCD 2015年第10期690-694,共5页
A rapid and accurate high performance liquid chromatography tandem mass spectrometry(HPLS-MS) method was established for quantification of chlorpromazine in pork. The porcine samples were pretreated with acetonitril... A rapid and accurate high performance liquid chromatography tandem mass spectrometry(HPLS-MS) method was established for quantification of chlorpromazine in pork. The porcine samples were pretreated with acetonitrile to precipitate proteins and followed by extraction with tert--butyl methyl ether(TBME). The separation was performed on a 5 μm Agilent XDB--C18 column with gradient elution. The mobile phase A was 0.01 mol/L ammonium formate in water and mobile phase B was acetonitrile. The flow rate was at 0.8 mL/min. Quantification was performed on a triple-quadrupole tandem mass spectrometer using the multiple selected reaction monitoring(MRM) mode. Transition of m/z +319.1 to 58.1 was used for the quantification of chlorpromazine. The method was validated at the concentration range of 0.4040 μg/kg to 8.080 μg/kg for chlorpromazine with correlation coefficient of 0.9999. The spiked recoveries were more than 80.0% and the limit of detection(LOD) was 0.052 μg/kg. The developed method, which offers advantages of convenience, rapid, specificity and higher sensitivity, can be used for determination of chlorpromazine hydrochloride in porcine muscles. 展开更多
关键词 high performance liquid chromatography-tandem mass spectrometry Chlorpromazine hydrochloride Porcine muscle Residual quantification
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高效液相色谱-串联四极杆质谱法测定人参组培不定根中11种皂苷成分
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作者 董喆 王玉梅 +3 位作者 孙姗姗 曹进 李梦怡 高飞 《化学分析计量》 CAS 2024年第10期55-62,共8页
建立高效液相色谱-串联四极杆质谱(HPLC-MS/MS)法定量分析人参组培不定根中11种皂苷成分。样品经粉碎研磨,以70%甲醇水溶液为溶剂进行超声提取,离心过滤后测定。采用C_(18)色谱柱(100 mm×2.1 mm,1.8μm),用水和乙腈进行梯度洗脱,... 建立高效液相色谱-串联四极杆质谱(HPLC-MS/MS)法定量分析人参组培不定根中11种皂苷成分。样品经粉碎研磨,以70%甲醇水溶液为溶剂进行超声提取,离心过滤后测定。采用C_(18)色谱柱(100 mm×2.1 mm,1.8μm),用水和乙腈进行梯度洗脱,流量为0.3 mL/min,柱温为35℃。质谱采用电喷雾电离源,负离子扫描,多反应监测模式进行检测。11种皂苷的质量浓度在0.1~10μg/mL(Rb1为0.2~10μg/mL)范围内和响应强度线性相关,相关系数均大于0.995,各皂苷的定量限为0.001~0.010 g/kg,加标回收率为90.43%~97.82%,相对标准偏差为1.93%~6.33%(n=6)。该方法操作简单,分析时间短,灵敏度高,准确可靠,适用于人参组培不定根中多种皂苷类成分的同时测定。 展开更多
关键词 高效液相色谱-串联四极杆质谱法 人参组培不定根 皂苷
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高效液相色谱-串联质谱法检测牛组织和奶中咪多卡残留的研究
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作者 白玉惠 孙红洋 +3 位作者 张骊 朱馨乐 沈昕 黄耀凌 《中国兽药杂志》 2024年第4期69-75,共7页
建立了一种检测牛组织和牛奶中咪多卡残留检测的高效液相色谱-串联质谱法。牛组织(肌肉、肝脏、肾脏、脂肪)和奶在NaAc缓冲体系中酶解,经HCl溶液提取,WCX固相萃取柱净化,以0.3%甲酸水溶液(含20 mM甲酸铵)和0.3%甲酸乙腈为流动相进行梯... 建立了一种检测牛组织和牛奶中咪多卡残留检测的高效液相色谱-串联质谱法。牛组织(肌肉、肝脏、肾脏、脂肪)和奶在NaAc缓冲体系中酶解,经HCl溶液提取,WCX固相萃取柱净化,以0.3%甲酸水溶液(含20 mM甲酸铵)和0.3%甲酸乙腈为流动相进行梯度洗脱,在HILIC色谱柱上分离,在电喷雾正离子(ESI^(+))模式下,用多反应监测(MRM)模式检测,同位素内标法定量。结果表明:咪多卡在2.5~1000 ng/mL的浓度范围内呈现良好线性关系,相关系数(R^(2))大于0.99;咪多卡在牛组织和奶中的检测限均为10μg/kg,定量限均为20μg/kg;咪多卡在牛组织和奶中20~4000μg/kg添加浓度水平上的回收率在70.9%~109%范围内;批内RSD在0.55%~9.59%之间,批间RSD在2.21%~12.1%之间。该方法具有灵敏度高、定量准确,重复性好等特点,可以满足牛组织和奶中咪多卡残留检测的要求。 展开更多
关键词 牛组织 牛奶 咪多卡 残留 高效液相色谱-串联质谱法
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配合饲料中64种药物超高效液相色谱-三重四极杆串联质谱检测方法的研究
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作者 陈海燕 陈娟 +4 位作者 李永琴 马春芳 张慧宁 杨俊华 杨奇 《畜牧与饲料科学》 2024年第3期11-19,共9页
[目的]建立同时检测配合饲料中64种药物的超高效液相色谱-三重四极杆串联质谱(ultra-high performance liquid chromatography-triple quadrupole tandem mass spectrometry,UHPLC-MS/MS)法,提高非法添加物的检测效率。[方法]采用Waters... [目的]建立同时检测配合饲料中64种药物的超高效液相色谱-三重四极杆串联质谱(ultra-high performance liquid chromatography-triple quadrupole tandem mass spectrometry,UHPLC-MS/MS)法,提高非法添加物的检测效率。[方法]采用Waters HSS T3型色谱柱(2.1 mm×100 mm,1.8μm)进行分离,流动相A为0.1%甲酸水溶液,流动相B为含0.1%甲酸的乙腈溶液,梯度洗脱,流速为0.40 mL/min,进样量为2μL;采用电喷雾离子源正离子扫描模式进行检测,多反应监测模式进行信号采集。比较4种样品提取溶剂以及2种固相萃取柱处理对目标药物的回收率,确定样品前处理的最佳方法。利用建立的UHPLC-MS/MS法对宁夏回族自治区不同来源的100批次配合饲料样品进行64种药物检测。[结果]配合饲料样品均质后,用含0.2%甲酸的乙腈水溶液(乙腈∶水=8∶2,V/V)提取,利用Oasis PRiME HLB型固相萃取柱对样品净化,多数目标药物的回收率在60%以上。64种药物在浓度为5.0~200.0μg/L的范围内线性关系良好,相关系数(R)均大于0.99;不同药物的定量限在5.0~10.0μg/kg;阳性添加5.0、20.0、50.0μg/kg 3个浓度的平均回收率在41.00%~120.49%,批内相对标准偏差(RSD)在0.54%~15.94%,批间RSD在1.25%~13.64%。在100个批次的配合饲料样品中均未检出目标药物。[结论]建立的UHPLC-MS/MS法线性关系良好、回收率高、精密度好,具有较高的重现性和较好的可操作性,可用于配合饲料中非法添加64种药物的筛查。 展开更多
关键词 配合饲料 超高效液相色谱-三重四极杆串联质谱法 非法添加 兽药
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超高效液相色谱-串联质谱法同时测定当归9种真菌毒素
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作者 李玉芳 焦洁 +5 位作者 黄铮 肖锋 黄远飞 王青 柳利龙 张环 《寒旱农业科学》 2024年第10期974-980,共7页
通过优化液相色谱条件和质谱条件等,建立超高效液相色谱-串联质谱法(UPLC-MS/MS)测定当归中药材中9种真菌毒素的检测方法。样品经70%甲醇溶液超声提取,经固相萃取柱净化;采用流动相A:2 mmol/L甲酸铵0.1%甲酸水溶液;流动相B:甲醇,经C18... 通过优化液相色谱条件和质谱条件等,建立超高效液相色谱-串联质谱法(UPLC-MS/MS)测定当归中药材中9种真菌毒素的检测方法。样品经70%甲醇溶液超声提取,经固相萃取柱净化;采用流动相A:2 mmol/L甲酸铵0.1%甲酸水溶液;流动相B:甲醇,经C18色谱柱分离后注入质谱仪,电喷雾电离源(ESI)和多反应监测模式(MRM)进行检测,基质外标法定量。经方法学验证,9种真菌毒素标准曲线线性关系良好(R^(2)>0.9950),方法的检出限0.04~1.43μg/kg,定量限0.12~4.75μg/kg,高、中、低3个浓度加标回收率为77.8%~113.6%,测定结果的相对标准偏差为0.2%~17.7%。该检测方法应用于72批当归样品9种真菌毒素同时检测,2批当归样品检出真菌毒素,检出率为2.8%,样品中主要的污染真菌毒素为黄曲霉毒素B_(1)(AFTB_(1))、黄曲霉毒素B2(AFTB_(2))、黄曲霉毒素G_(1)(AFTG_(1))。本研究建立的方法具有预处理简便、经济等优点,适用于当归样品9种真菌毒素的快速检测。 展开更多
关键词 当归 中药材 真菌毒素 超高效液相色谱-串联质谱法 方法验证
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UPLC-MS/MS法检测3种食品中松仁过敏原
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作者 宁亚维 周泓鑫 +4 位作者 杨正 马俊美 刘茁 张岩 李强 《食品科学》 EI CAS CSCD 北大核心 2024年第1期247-253,共7页
基于食品基质中松仁过敏原Pin k 2建立了一种超高效液相色谱-串联质谱法。将松仁经过研磨、脱脂、浸提、酶解后经Easy-nLC 1000-QExactive高分辨质谱仪进行分离分析,结合Uniprot蛋白数据库以及ProteinPilotTM软件对质谱图进行数据处理,... 基于食品基质中松仁过敏原Pin k 2建立了一种超高效液相色谱-串联质谱法。将松仁经过研磨、脱脂、浸提、酶解后经Easy-nLC 1000-QExactive高分辨质谱仪进行分离分析,结合Uniprot蛋白数据库以及ProteinPilotTM软件对质谱图进行数据处理,经BLAST验证特异性,最终筛选3条松仁特异性肽段。方法学验证结果表明,方法在0.001~50mg/mL范围内线性关系良好,定量限为1mg/kg;在饼干、巧克力和饮料3种空白基质中的平均回收率为88.50%~107.57%,相对标准偏差不高于6.08%,基质效应为89.77%~96.13%。该方法具有灵敏度高、特异性好的优势,可应用于饼干、巧克力、饮料等食品样品中松仁过敏原的检测,为我国食品标签真实性检验及食品中隐性过敏原的检测提供技术支持。 展开更多
关键词 松仁 过敏原 超高效液相色谱-串联质谱法 检测
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淡竹叶多酚的提取纯化工艺优化、组分分析及体外抗氧化活性研究 被引量:1
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作者 周文月 文语佳 +2 位作者 周森林 杨明龙 时政 《食品安全质量检测学报》 CAS 2024年第1期254-263,共10页
目的确定淡竹叶多酚提取纯化工艺,分析主要成分及体外抗氧化活性。方法采用超声辅助提取淡竹叶多酚,通过响应面实验确定最佳提取条件。选取适合淡竹叶多酚纯化的大孔树脂,对纯化工艺参数进行优化。通过高效液相色谱-质谱法(high perform... 目的确定淡竹叶多酚提取纯化工艺,分析主要成分及体外抗氧化活性。方法采用超声辅助提取淡竹叶多酚,通过响应面实验确定最佳提取条件。选取适合淡竹叶多酚纯化的大孔树脂,对纯化工艺参数进行优化。通过高效液相色谱-质谱法(high performance liquid chromatography-mass spectrometry,HPLC-MS)鉴定淡竹叶多酚的主要成分,并评价其体外抗氧化活性。结果淡竹叶多酚的最佳提取工艺参数为:乙醇体积分数60%、超声功率500 W、料液比1:25(g/mL)、超声时间24 min及超声温度59℃,该条件下淡竹叶多酚提取量为8.01 mg/g。淡竹叶多酚纯化工艺参数为:上样质量浓度6 mg/mL、pH 4、流速2 mL/min、解吸液为70%乙醇、解吸体积90 mL,纯化后的淡竹叶多酚纯度由12.86%提高到76.18%。通过HPLC-MS鉴定出16种酚类成分,且纯化后多酚有较高的抗氧化活性。结论本研究得到了淡竹叶多酚提取纯化工艺,得到的多酚纯化物有明显的抗氧化活性。 展开更多
关键词 淡竹叶 多酚 响应面法 纯化工艺 抗氧化活性 高效液相色谱-质谱法
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平衡透析法测定加米霉素与猪、牛和羊的血浆蛋白结合率
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作者 姚鑫 叶昕熠 +3 位作者 张鑫鑫 符文真 刘雅红 周宇峰 《中国兽医杂志》 CAS 北大核心 2024年第10期81-87,共7页
为测定加米霉素与常见家畜的血浆蛋白结合率(PPBR),本试验建立猪、牛和羊血浆中加米霉素的高效液相色谱-串联质谱检测方法,并对该方法的专属性、检测限、定量限、标准曲线、提取回收率和精密度进行考察。采用平衡透析法测定不同浓度(0.1... 为测定加米霉素与常见家畜的血浆蛋白结合率(PPBR),本试验建立猪、牛和羊血浆中加米霉素的高效液相色谱-串联质谱检测方法,并对该方法的专属性、检测限、定量限、标准曲线、提取回收率和精密度进行考察。采用平衡透析法测定不同浓度(0.1、0.5和2.5μg/mL)加米霉素与猪、牛和羊的PPBR。结果显示,在考察浓度范围内,加米霉素在猪、牛和羊血浆中的专属性较好,检测限和定量限分别为0.5和1.0 ng/mL,标准曲线呈现良好的线性关系(r>0.997)。加米霉素在猪、牛和羊血浆中的提取回收率介于91.2%~107.8%,日内和日间精密度相对标准偏差(RSD)分别小于6.59%和9.16%。加米霉素与猪、牛和羊的平均PPBR分别为(21.86±4.19)%、(27.51±6.95)%和(19.64±3.58)%,且在考察的浓度范围内无浓度依赖特征。本试验所建方法准确可靠,可用于测定加米霉素与猪、牛和羊的PPBR。本试验结果可为加米霉素的药物代谢动力学研究及其在兽医临床中的科学用药提供参考依据。 展开更多
关键词 加米霉素 血浆蛋白结合率 平衡透析法 高效液相色谱-串联质谱(HPLC-MS/MS)
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清瘟护肺颗粒化学成分研究
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作者 龙凯花 刘静 +4 位作者 曹利平 刘满军 刘洋 杜霞 张红 《中国药业》 CAS 2024年第10期37-47,共11页
目的研究清瘟护肺颗粒的化学成分。方法查阅中国知网、PubMed、Web of Science等数据库,检索该制剂组方药材化学成分的相关文献,结合文献报道和ChemicalBook数据库信息,建立化学成分数据库。采用超高效液相色谱-四极杆/静电场轨道阱高... 目的研究清瘟护肺颗粒的化学成分。方法查阅中国知网、PubMed、Web of Science等数据库,检索该制剂组方药材化学成分的相关文献,结合文献报道和ChemicalBook数据库信息,建立化学成分数据库。采用超高效液相色谱-四极杆/静电场轨道阱高分辨质谱(UHPLC-Q Exactive Focus MS/MS)法分析制剂的图谱数据,并以Xcalibur 4.0软件拟合分子式,与自建数据库信息进行匹配,初步推测分子式信息,与ChemicalBook或ChemSpider数据库比对,推测化学成分结构。结果共鉴定出158个化学成分,包括苷类36个,黄酮类29个,苯丙素类28个,有机酸类18个,萜类17个,色原酮类8个,其他类22个。结论所建立的方法可系统、准确、快速地定性分析清瘟护肺颗粒中的化学成分。 展开更多
关键词 清瘟护肺颗粒 超高效液相色谱-四极杆/静电场轨道阱高分辨质谱法 化学成分 结构鉴定
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超高效液相色谱-串联质谱法测定奈玛特韦及利托那韦血药浓度
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作者 范菁 唐昊翔 +3 位作者 王银辉 范炜斌 谢姣 林彬 《医药导报》 北大核心 2024年第2期190-195,共6页
目的建立一种具有高灵敏度、高稳定性并且通用性强的能同时测定人血浆中奈玛特韦和利托那韦血药浓度的超高效液相色谱-串联质谱法。方法分离色谱柱采用ACQUITY UPLC BEH C_(18)柱(2.1 mm×50 mm,1.7μm),采用梯度洗脱,流动相为100%... 目的建立一种具有高灵敏度、高稳定性并且通用性强的能同时测定人血浆中奈玛特韦和利托那韦血药浓度的超高效液相色谱-串联质谱法。方法分离色谱柱采用ACQUITY UPLC BEH C_(18)柱(2.1 mm×50 mm,1.7μm),采用梯度洗脱,流动相为100%乙腈-0.1%甲酸,流速为0.3 mL·min^(-1),柱温为45℃,进样量为2μL。以电喷雾离子(ESI+)作为离子源,多反应监测模式扫描(奈玛特韦m/z 500.20→319.10,奈玛特韦-D_(9)m/z 508.59→328.10,利托那韦m/z 721.30→426.10,^(13)C,^(2)H_(3-)利托那韦m/z 725.30→426.10)。选择2023年1月于长兴县人民医院接受奈玛特韦/利托那韦治疗的新型冠状病毒感染患者30例,测定其用药3 d后的奈玛特韦和利托那韦稳态谷浓度。结果人血浆中奈玛特韦及利托那韦的线性范围分别为0.10~10.00(R^(2)=0.9972)和0.05~5.00μg·mL^(-1)(R^(2)=0.9952)。奈玛特韦和利托那韦的回收率均>90%,批内以及批间精密度的相对标准差(RSD)均<10%。另外,奈玛特韦和利托那韦回收率范围为91.5%~97.0%,基质效应范围为92.4%~97.7%。临床结果表明新型冠状病毒感染患者奈玛特韦和利托那韦血药浓度个体差异性很大。结论该研究建立的同时测定人血浆中奈玛特韦和利托那韦浓度的检测方法操作方便、专属性强、准确度及精密度高,适用于临床患者奈玛特韦和利托那韦血药浓度监测。 展开更多
关键词 奈玛特韦 利托那韦 超高效液相色谱-串联质谱法 新型冠状病毒
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三子养亲汤中11种成分含量同时测定及其胰脂肪酶抑制作用研究
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作者 张昊 巩丽丽 +2 位作者 王婧毅 李海超 齐冬梅 《中成药》 CAS CSCD 北大核心 2024年第6期1788-1793,共6页
目的同时测定三子养亲汤中3,6′-二芥子酰基蔗糖、西伯利亚远志糖A5、西伯利亚远志糖A6、阿魏酸、芥子酸、咖啡酸、木犀草素、原告依春、芹菜素、异鼠李素、原儿茶醛的含量,并考察其对胰脂肪酶的抑制作用。方法高效液相色谱-串联三重四... 目的同时测定三子养亲汤中3,6′-二芥子酰基蔗糖、西伯利亚远志糖A5、西伯利亚远志糖A6、阿魏酸、芥子酸、咖啡酸、木犀草素、原告依春、芹菜素、异鼠李素、原儿茶醛的含量,并考察其对胰脂肪酶的抑制作用。方法高效液相色谱-串联三重四级杆质谱(HPLC-QQQ-MS/MS)分析采用Halo-C 18色谱柱(2.1 mm×100 mm,2.7μm);流动相水(含0.05%甲酸)-乙腈(含0.05%甲酸),梯度洗脱;体积流量0.3 mL/min;柱温25℃;电喷雾离子源;负离子扫描;多反应监测模式。采用分子对接进行模拟,对硝基苯酚法评价抑制作用。结果11种成分在各自范围内线性关系良好(R^(2)>0.9920),平均加样回收率85.79%~117.52%,RSD 0.78%~3.73%。3,6′-二芥子酰基蔗糖、咖啡酸、芥子酸和原儿茶醛与胰脂肪酶具有良好的亲和力,三子养亲汤、咖啡酸、芥子酸、原儿茶醛IC_(50)值分别为41.16 mg/mL、4.006 mmol/L、6.798 mmol/L、10.48 mmol/L。结论该方法稳定可靠,可为具有胰脂肪酶活性抑制作用的三子养亲汤质量控制提供理论基础。 展开更多
关键词 三子养亲汤 化学成分 含量测定 胰脂肪酶 高效液相色谱-串联三重四级杆质谱(HPLC-QQQ-MS/MS) 分子对接 对硝基苯酚法
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基于干燥工艺对比两种寄主肉苁蓉中苯乙醇苷类成分含量
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作者 高培文 郭晔红 +2 位作者 赵法法 张丹 张芳明 《食品与发酵工业》 CAS CSCD 北大核心 2024年第20期273-278,共6页
利用超高效液相色谱-三重四极杆串联质谱联用法(ultra-high performance liquid chromatography-triple quadrupole mass spectrometry, UPLC-QQQ-MS)比较2种寄主肉苁蓉经过不同干燥处理后的10种苯乙醇苷类成分含量。将肉苁蓉干燥品粉碎... 利用超高效液相色谱-三重四极杆串联质谱联用法(ultra-high performance liquid chromatography-triple quadrupole mass spectrometry, UPLC-QQQ-MS)比较2种寄主肉苁蓉经过不同干燥处理后的10种苯乙醇苷类成分含量。将肉苁蓉干燥品粉碎,粉末过60目筛,用50%(体积分数)甲醇溶解后超声提取,用Agilent Eclipse Plus C18柱(2.1 mm×150 mm, 1.8μm)分离,以A相(0.1%甲酸水溶液)-B(乙腈)相作为流动相进行梯度洗脱,利用电喷雾离子源,在UPLC-QQQ-MS的动态多反应模式下检测。结果表明,不同干燥处理的寄主肉苁蓉苯乙醇苷类成分含量具有明显差异,冷冻干燥处理所得的肉苁蓉中10种苯乙醇苷类含量最高,其次为80℃烘干样品。虽然冷冻干燥对于肉苁蓉所保留10种苯乙醇苷类成分最高,但基于大规模生产考虑,80℃烘干更具有经济效益。 展开更多
关键词 超高效液相色谱-三重四极杆串联质谱联用法 肉苁蓉 梭梭 四翅滨藜 苯乙醇苷类 干燥方式
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QuEChERS-高效液相色谱-串联质谱法检测甘薯和土壤中烯效唑残留的方法研究
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作者 左仁芳 戴桂金 +6 位作者 王妙 张玉涵 罗杰 熊浩 刘志邦 陈武瑛 张卓 《湖南农业科学》 2024年第5期90-95,共6页
采用改良的QuEChERS方法进行前处理,建立了甘薯和土壤中烯效唑残留的QuEChERS-高效液相色谱-串联质谱检测方法。样品用含0.1%乙酸的乙腈振荡提取,经C18净化剂进行基质净化,采用C18反相色谱柱分离,进行LC-MS/MS检测。结果表明:烯效唑在0.... 采用改良的QuEChERS方法进行前处理,建立了甘薯和土壤中烯效唑残留的QuEChERS-高效液相色谱-串联质谱检测方法。样品用含0.1%乙酸的乙腈振荡提取,经C18净化剂进行基质净化,采用C18反相色谱柱分离,进行LC-MS/MS检测。结果表明:烯效唑在0.0005~1.0 mg/L浓度范围内,质量浓度与对应的峰面积间呈良好的线性关系,相关系数为0.9951~0.9959;在0.002、0.02、0.20 mg/kg 3个添加水平下,烯效唑在甘薯和土壤中的平均回收率为90.3%~106.7%,相对标准偏差为0.6%~3.6%,方法定量限为0.002 mg/kg。该方法方便快捷、精准定量、检测灵敏,适用于甘薯和土壤样品中烯效唑的检测。 展开更多
关键词 烯效唑 甘薯 高效液相色谱-串联质谱 残留 方法
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Detection of Endocrine Disruptors in Water around Landfills
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作者 Dandan LIU Qing LI +4 位作者 Yaohong LIU Sha FENG Tao MO Zheng LIU Xiaonan ZOU 《Agricultural Biotechnology》 2024年第1期66-70,73,共6页
[Objectives]This study was conducted to explore the occurrence levels of endocrine disruptors(EDCs)in rural areas around a county landfill in Tongren City.[Methods]The water around the landfill was sampled and analyze... [Objectives]This study was conducted to explore the occurrence levels of endocrine disruptors(EDCs)in rural areas around a county landfill in Tongren City.[Methods]The water around the landfill was sampled and analyzed.A solid-phase extraction and high performance liquid chromatography-tandem mass spectrometry(SPE-UPLC-MS/MS)method was established for the determination of 27 EDCs.After the HLB solid-phase extraction column was activated,a water sample,which was adjusted with phosphoric acid to a pH of 2(±0.5)and added with 500 mg of disodium EDTA,was loaded,and 5 ml of water and 20%methanol water was added for washing.Next,10 ml of elution solution was added for elution,and the collected eluate was evaporated under reduced pressure at 40℃to near dryness,and 1 ml of reconstitution solution was added to a constant volume.An ACQUITY UPLC BEH C18(100×2.1 mm,2.6μm)chromatographic column was adopted for LC separation by gradient elution with pure water solution-acetonitrile as the mobile phase.For MS detection,the MRM mode was adopted for collection,and the positive and negative ion modes were switched for simultaneous determination,and the internal standard method was used for quantification.[Results]The correlation coefficient R2 was greater than 0.99 in the linear range of each target substance.The limits of quantitation in the method were between 0.05 and 2.00 ng/L,and the recoveries ranged from 75.3%to 105.7%.[Conclusions]The method has high sensitivity,good accuracy and strong practical value. 展开更多
关键词 LANDFILL Endocrine disruptor Solid phase extraction high performance liquid chromatography-tandem mass spectrometry
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Study on Detection of Antibiotic Contents in Water around Landfill Sites
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作者 Sha FENG Dandan LIU +4 位作者 Juan LUO Qing LI Tao MO Zheng LIU Xiaonan ZOU 《Agricultural Biotechnology》 2024年第2期33-37,共5页
[Objectives] An ultra performance liquid chromatography-tandem mass spectrometry (UPLC-MS/MS) method was established for simultaneous determination of 26 antibiotics in the water around landfills. [Methods] After an H... [Objectives] An ultra performance liquid chromatography-tandem mass spectrometry (UPLC-MS/MS) method was established for simultaneous determination of 26 antibiotics in the water around landfills. [Methods] After an HLB solid-phase extraction column was activated, and a water sample, which was adjusted with phosphoric acid to a pH of (2±0.5) and added with 500 mg of disodium EDTA, was loaded, and 5 ml of water and 20% methanol water was added for washing. Next, 10 ml of elution solution was added for elution, and the collected eluate was evaporated under reduced pressure at 40 ℃ to near dryness, and 1 ml of reconstitution solution was added to a constant volume. An ACQUITY UPLC BEH C18 (100 mm×2.1 mm, 2.6 μm) chromatographic column was adopted for LC separation by gradient elution with 0.1% formic acid aqueous solution-acetonitrile as the mobile phase. For MS detection, the MRM mode was adopted for collection, and the positive and negative ion modes were switched for simultaneous determination, and the internal standard method was used for quantification. [Results] The correlation coefficient R2 was greater than 0.99 in the linear range of each target substance. The limits of detection ranged from 0.15 to 3.00 ng/L, and the limits of quantitation were between 0.80 and 10.00 ng/L, and the recoveries ranged from 77.9% to 104.85%. [Conclusions] The method has high sensitivity, good accuracy and strong practical value. 展开更多
关键词 LANDFILL ANTIBIOTICS Ultra high performance liquid chromatography-tandem mass spectrometry
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高效液相色谱法同时测定淋洗类化妆品中7种异噻唑啉酮类防腐剂及质谱确证
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作者 陈岑 崔邶周 +2 位作者 张丽媛 颜琳琦 程巧鸳 《日用化学工业(中英文)》 CAS 北大核心 2024年第10期1268-1275,共8页
建立了同时检测淋洗类化妆品中7种异噻唑啉酮类防腐剂的高效液相色谱分析方法及液相色谱-串联质谱确证方法。膏霜乳和液体两种不同基质类型的化妆品样品分别经甲醇超声提取,提取液以离心处理后,取上清液经微孔滤膜过滤后测定。经CAPCELL... 建立了同时检测淋洗类化妆品中7种异噻唑啉酮类防腐剂的高效液相色谱分析方法及液相色谱-串联质谱确证方法。膏霜乳和液体两种不同基质类型的化妆品样品分别经甲醇超声提取,提取液以离心处理后,取上清液经微孔滤膜过滤后测定。经CAPCELL PAK C_(18)MGIII(4.6 mm×250 mm,5μm)色谱柱分离,以甲醇和0.1%磷酸水溶液为流动相梯度洗脱,流速1.0 ml/min,柱温40℃。检测波长为275,282,和319 nm。以高效液相色谱法的结果进行定性筛查,并采用标准曲线法定量,以液相色谱-串联质谱法的结果进行确证。结果表明,7种异噻唑啉酮类防腐剂在0.1~50 mg/L质量浓度范围内线性关系良好,相关系数均≥0.9999。在低、中、高3种加标浓度水平下,平均加标回收率分别为97.5%~109.9%(膏霜乳)和95.6%~103.6%(液体);相对标准偏差(RSD)小于3.0%,检出限为0.05~0.11 mg/kg。该方法具有简单、快速、准确性好的特点,适用于淋洗类化妆品中7种异噻唑啉酮类防腐剂的含量测定及质谱确证。 展开更多
关键词 淋洗类化妆品 高效液相色谱法 质谱确证 异噻唑啉酮类防腐剂
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高效液相色谱-串联质谱法测定玉米蛋白粉中黄曲霉毒素B_(1)测量不确定度评定
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作者 王鑫 张凤枰 杨娟 《中国粮油学报》 CAS CSCD 北大核心 2024年第5期181-188,共8页
采用GUM法和Top-down法对高效液相-串联质谱法测定玉米蛋白粉中的黄曲霉毒素B_(1)测量不确定度进行评定。通过比较2种方法的评定过程和评定结果发现,Top-down法在简化评定步骤、保证评定结果可靠性的前提下,能够充分利用实验室检测数据... 采用GUM法和Top-down法对高效液相-串联质谱法测定玉米蛋白粉中的黄曲霉毒素B_(1)测量不确定度进行评定。通过比较2种方法的评定过程和评定结果发现,Top-down法在简化评定步骤、保证评定结果可靠性的前提下,能够充分利用实验室检测数据和质量控制数据,引入检测人员变动、检测仪器更换等带来的不确定度,是一种客观、高效的不确定度评定方法,为饲料中黄曲霉毒素B_(1)检测数据准确溯源提供参考。 展开更多
关键词 高效液相色谱-串联质谱法 测量不确定度 GUM法 Top-down法 黄曲霉毒素B_(1)
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