Simultaneous quantification of several classes of antibiotics in water,sediments, and fish muscles by liquid chromatography–tandem mass spectrometry

Precise and sensitive methods for the simultaneous determination of different classes of antibiotics, including sulphonamides, fluoroquinolones, macrolides, tetracyclines, and trimethoprim in surface water, sediments, and fish muscles were developed. In water samples, drugs were extracted with solid-phase extraction (SPE) by passing 1000 mL of water through hydrophilic lipophilic balanced (HLB) SPE cartridges. Sediment samples were solvent-extracted, followed by tandem SPE (strong anion exchange (SAX) + HLB) clean-ups. Fish muscles were extracted by a mixture of acetonitrile and citric buffer (80:20, v/v) solution, and cleaned by SPE. Liquid chromatography–tandem mass spectrometry (LC-MS/MS) with multiple reaction monitoring (MRM) detection was employed to quantify all compounds. The recoveries for the antibiotics in the spiked water, sediment, and fish samples were 60.2%–95.8%, 48.1%–105.3%, and 59.8%–103.4%, respectively. The methods were applied to samples taken from Dianchi Lake, China. It showed that concentrations of the detected antibiotics ranged from limits of quantification (LOQ) to 713.6 ng·L^-1 (ofloxacin) in surface water and from less than LOQ to 344.8 μg·kg^-1 (sulphamethoxazole) in sediments. The number of detected antibiotics and the overall antibiotic concentrations were higher in the urban area than the rural area, indicating the probable role of livestock and human activities as important sources of antibiotic contamination. In fish muscles, the concentration of norfloxacin was the highest (up to 38.5 μg·kg^-1), but tetracyclines and macrolides were relatively low. Results showed that the methods were rapid and sensitive, and capable of determining several classes of antibiotics from each of the water, sediment, and fish matrices in a single run.     

QuEChERS-超高效液相色谱-串联质谱法测定鱼血清中的精神活性物质

本文建立了一种同时测定鱼血清中19种精神活性物质的分析方法.该方法基于QuEChERS方法对样品进行提取和净化,待测物采用超高效液相色谱-串联质谱法(UPLC-MS/MS)进行分析,检测的19种精神活性物质均采用同位素内标法定量.该方法的方法检测限(MDL)范围为0.02-0.06 ng.mE-1,基质效应处于76.7...     

高效液相色谱-串联质谱法同时检测水体中26种药物及个人护理品

通过优化固相萃取条件和高效液相色谱-串联质谱参数,建立了可以同时检测地表水和地下水中26种典型药物及个人护理品(pharmaceuticals and personal care products,PPCPs),包括磺胺类、大环内酯类、喹诺酮类、酰胺醇类、精神类、消炎止痛类以及个人护理品的检测方法.通过将水样pH值调节...     

高效液相色谱-质谱联用法测定饮用水中的五氯苯酚

建立了高效液相色谱-质谱联用法检测饮用水中五氯苯酚(PCP)。选用ZORBAXXDB-C18柱(50mm×2.1mm,3.5μm)为分析柱,流动相为V(甲醇):V(纯水)=88:12,流量为200μL·min-1;质谱条件选用气动辅助电喷雾离子源(ESI),检测方式为负离子多离子反应检测(MRM);PCP标准曲线线形范围为0.1～100μg·L-1;方法加标回收率达到90%以上;相对标准偏差为2.31%～2.92%(n=5);方法检测低限为0.1μg·L-1。结果表明该方法快速、简便、准确、灵敏、特异,适用于饮用水中PCP残留的测定。     

高效液相色谱-质谱联用法测定饮用水中的五氯苯酚

建立了高效液相色谱-质谱联用法检测饮用水中五氯苯酚（PCP）。选用ZORBAXXDB-C18柱（50mm×2．1mm,3．5μm）为分析柱,流动相为V（甲醇）：V（纯水）=88：12,流量为200μL·min-1;质谱条件选用气动辅助电喷雾离子源（ESI）,检测方式为负离子多离子反应检测（MRM）;PCP标准曲线线形范围为0．1～100μg·L-1;方法加标回收率达到90％以上;相对标准偏差为2-31％-2．92％（n=5）;方法检测低限为0．1μg·L-1。结果表明该方法快速、简便、准确、灵敏、特异,适用于饮用水中PCP残留的测定。     

超高效液相色谱串联质谱法检测鱼体中的全氟化合物

采用超高效液相色谱-串联质谱联用法(UPLC-ESI-MS/MS),建立了检测1种贝类和2种鱼类的肌肉组织中11种全氟化合物(PFCs)的分析方法.采用碱液消解做为样品前处理法,选Carbon/NH2双层SPE小柱做为净化小柱,并以ACQUITY UPLC BEH C18为分析柱,甲醇和2 mmol.L-15%甲醇乙酸铵溶液为梯度淋洗液.所选定的11种全氟化合物在6 min内就可以达到良好分离,外标法定量.平均回收率在72.1%—93.6%之间,相对标准偏差在0.6%—9.5%之间,实际检出限在3.4—26.7 pg.g-1.     

通过式固相萃取/超高效液相色谱-串联质谱法测定蔬菜中18种农药残留

建立了超高效液相色谱-串联质谱(UPLC-MS;MS)快速测定蔬菜中18种农药残留的方法.样品经乙腈提取后,经Oasis PRiME HLB固相萃取柱净化,采用ACQUITY UPLC HSS T3 C18(50 mm×2.1 mm,1.8μm)色谱柱进行分离,以0.1%甲酸水溶液和乙腈作为流动相进行梯度洗脱.采用电喷雾电离源、正离子模式下以多反应监测(MRM)进行定性和定量分析.结果表明,18种农药在0.5—50μg·L^-1范围内线性关系良好(r2>0.995),方法最低检出限为0.4—1.5μg·kg^-1,最低定量限为1.4—5.0μg·kg^-1.在韭菜、芹菜、番茄、白菜基质中,5、10、50μg·kg^-1添加水平下的加标回收率为60.2%—126.9%,相对标准偏差(RSD)为0.4%—21.6%(n=3).     

基于液相色谱法分析水环境中大环内酯类抗生素污染的研究进展

大环内酯抗生素广泛使用,在水环境中的残留越来越引起世界关注.本文综述了国内外基于液相色谱技术分析水环境中大环内酯的方法,比较不同预处理法以及分析方法的灵敏度和检出限.固相萃取法可以同时富集和净化,消耗试剂少,方便,野外操作可行,是理想的预处理技术.液相色谱串联质谱技术选择性好、特异性高、灵敏度高,可以检测浓度低于ng.L-1的目标物,是一种可靠理想的分析方法.最后对大环内酯分析研究进行了展望.     

超高效液相色谱-串联质谱法同时测定环境水样中的15种抗生素

采用固相萃取/超高效液相色谱-串联质谱法,建立了水样中磺胺类、四环素类、氟喹诺酮类、大环内酯类和氯霉素类15种抗生素的同时测定方法.水样经HLB固相萃取柱富集,ACQUITY UPLC BEH C_(18)色谱柱分离,以乙腈和5 mmol·L~(-1)乙酸铵溶液(含0.1%甲酸)为流动相梯度洗脱,电喷雾离子源-串联质谱多反应监测模式检测.结果表明,同时测定15种抗生素的线性范围为5—100μg·L~(-1)(相关系数均大于0.997),检出限为2.1—22.0 ng·L~(-1),定量限为6.9—71.8 ng·L~(-1);空白水样在加标水平为5、10、20μg·L~(-1)时,抗生素的回收率为50.1%—109.0%,相对标准偏差为0.4%—8.5%(n=7).用本文建立的方法检测某农业小流域环境水样,发现5类抗生素可被不同程度检出,浓度范围为0.1—106.2 ng·L~(-1).     

基于分散固相萃取-超高效液相色谱串联质谱法测定沉积物中大环内酯类抗生素

采用分散固相萃取与超高效液相色谱串联质谱技术,建立了快速测定沉积物中9种大环内酯类抗生素(螺旋霉素、阿奇霉素、替米考星、竹桃霉素、红霉素、泰乐菌素、吉他霉素、罗红霉素和交沙霉素)的检测方法.沉积物经磷酸盐缓冲液和乙腈混合液浸提,再经过石墨化炭黑和C18硅胶分散固相萃取材料净化.采用超高效液相色谱串联质谱仪(UPLC-M...     

超高效液相色谱-三重四极杆串联质谱法测定蜂蜜中吡咯里西啶类生物碱

建立了蜂蜜中5种吡咯里西啶类生物碱的超高效液相色谱-串联质谱测定方法.蜂蜜样品用50%甲醇超声提取,强阳离子交换固相萃取柱净化富集,超高效液相色谱-三重四极杆串联质谱MRM模式检测,外标法定量.以Waters BEH C18(100 mm×2.1 mm,1.7μm)色谱柱分离,以含0.1%甲酸的乙腈和0.1%甲酸水溶液进行梯度洗脱.倒千里光碱、千里光宁、千里光菲啉和野百合碱在0.2—100.0μg·kg-1,克氏千里光宁在1.0—200.0μg·kg-1的浓度范围内各化合物线性关系良好,相关系数r均大于0.999,定量限在0.2—0.8μg·kg-1之间.在3个加标水平下,空白基质蜂蜜中的5种生物碱的平均回收率为82.0%—110.0%之间,相对标准偏差(RSD)小于12.5%.方法准确可靠,适合于蜂蜜中吡咯里西啶类生物碱的测定.     

超高效液相色谱/三重四极杆质谱-直接进样分析地表水中硝基酚类化合物

本文建立了一种使用岛津超高效液相色谱仪Nexera X2和三重四极杆质谱仪LCMS-8050联用直接进样分析水中硝基酚类化合物的方法.本方法可在5 min内完成3种硝基酚类化合物分析.采用内标法定量,方法线性范围为0.1—100.0μg·L~(-1),相关系数大于0.998,各浓度回读值准确度在85.8%—112.7%之间.3个浓度下保留时间和峰面积的相对标准偏差(RSD%)分别在0.10%—0.20%和0.85%—3.30%之间.进样2.0μL,方法检出限在0.022—0.034μg·L~(-1)之间,测定下限在0.088—0.136μg·L~(-1)之间.地表水3个不同浓度样品加标回收率在86.7%—94.5%之间.残留实验结果为阴性.     

固相萃取-高效液相色谱-串联质谱法测定地表水中40种抗生素

建立了固相萃取-高效液相色谱-串联质谱法(HLB-HPLC-MS9种氟喹诺酮类(QNs)、7种大环内酯类(MCs)、3种四环素类(TCs)、2种氯霉素类(CAPs)和4种其他类(Others)共40种抗生素的分析方法.通过重点优化水样不同pH值、乙二胺四乙酸二钠(Na2EDTA)加入量、色谱条件和质谱参数等确定了最佳分析条件.水样经HLB固相萃取柱富集净化,采用Agilent Zorbax Rrhd Eclipse Plus C18 (2.1 mm×50 mm,1.8μm)色谱柱分离,正、负离子模式分别采集,正离子模式采用0.2%甲酸-2 mmol乙酸铵水溶液和甲醇-乙腈(V/V,1∶1)作流动相梯度洗脱分离38种单体;负离子模式采用纯水和甲醇-乙腈(V/V,1∶1)作流动相梯度分离2种单体,多重反应监测模式分析,内标法定量.结果显示:目标分析物线性范围在1.00—200 ng·mL~(-1)之间,相关系数r2均大于0.99,方法检出限在0.002—0.270 ng·L~(-1)之间,地表水加标回收率在61.0%—149%之间,相对标准偏差(RSD)在1.2%—32%之间.方法成功应用于贵阳市南明河12个地表水分析,共检出34种抗生素,其中大环内酯类检出浓度最高,平均浓度为257 ng·L~(-1).     

Determination of pesticides in apples,grapes and apple juice from a Kosovo market by gradient liquid chromatography with tandem mass spectrometry

Apple, grape, and apple juice were analyzed for pesticides using a multireaction mode (MRM) method in samples taken from a Kosovo market. With this method it was possible to analyze about 100 pesticides in the ESI mode. In these samples some types of pesticides were found, but most of them did not exceed the maximum tolerance levels. In apple samples, six pesticides were detected but only three of them were in sufficient quantitites. Dimethoat was below the limit, while acephate and imazalil exceeded the limit. In grape and apple juice samples, all of pesticides which were found did not exceed the maximum tolerable limits.     

近岸海水中全氟化合物的液相色谱-离子阱质谱法测定

建立了利用高效液相色谱-电喷雾离子阱质谱(HPLC-ESI-IT-MS/MS)测定近岸海水中多种常见全氟化合物(PFCs)的分析方法.采用固相萃取法(SPE)对海水中的PFCs净化富集,用HPLC-ESI-IT-MS/MS多反应离子监测(MRM)模式对各组分(全氟己烷磺酸、全氟辛烷磺酸、全氟辛烷磺酰胺、全氟己酸、全氟庚酸、全氟辛酸、全氟壬酸、全氟癸酸、全氟十一酸、全氟十二酸)进行测定.在最佳实验条件下,采用基质匹配标准曲线法定量,以消除海水基质的影响,8种目标化合物的检出限介于0.50—1.00 ng·L-1,9种PFCs的回收率在71.0%—130.2%之间,能满足近岸海水中多种PFCs检测的要求.青岛沿岸表层海水样品测定结果显示,全部采样站点的海水样品中均检测到≥4种PFCs,说明青岛沿岸海水中已有一定程度的PFCs污染.     

Field evaluation and determination of four herbicides in a wheat ecosystem by a simple and versatile QuEChERS method with liquid chromatography-tandem mass spectrometry

Wheat products are consumed worldwide and every day; therefore, herbicides misuse in the wheat ecosystem has become a global food safety issue. Here, a simple and versatile method, QuEChERS (quick, easy, cheap, effective, rugged, and safe) with liquid chromatography-tandem mass spectrometry was developed to measure four herbicides in soil, wheat, and wheat straw – florasulam, carfentrazone-ethyl, fluroxypyr-meptyl, and fluroxypyr. By adjusting the amount of graphitized carbon black from 0 to 10 mg, the herbicides could be extracted with satisfactory recoveries of 80%–110%. Application of two water-dispersible granules showed first-order kinetics as well as half-lives between 1.2 and 5.1 d under open-field conditions. The dissipation kinetics of the four herbicides differed in the soil, wheat, and wheat straw, with residual concentrations in straw at 2 h after application being higher than in soil and faster degradation occurring in straw. The terminal residues in soil, wheat grain, and wheat straw were all below the maximum residue limits. The developed method was easy to handle and versatile; thus, it will facilitate regulation and inspection for possible misuse against Good Agriculture Practices. Moreover, the results of this study will contribute to global environmental protection as well as food safety issues.     

鱼体中有机微污染物的定量及筛查研究进展

化学品通过多种途径进入环境水体,可对水生生物及人体健康造成潜在风险.鱼类作为水环境污染物监测的指示生物,分析鱼体内有机微污染物的分布特征是评估水环境安全的重要方法.现有污染物种类繁多,且在生物体内存在降解转化的过程,基于靶向定量分析的监测方法难以系统、准确地评估鱼体中有机污染物的暴露特征.由于具有高分辨率、高质量精度、...     

加速溶剂萃取-固相萃取净化-超高效液相色谱串联质谱法测定土壤中11种全氟化合物

采用超高效液相色谱-串联质谱联用法（UPLC-ESI-MS/MS）,建立了分析土壤中11种全氟化合物（PFCs）的方法.以甲醇作为萃取剂,样品经加速溶剂萃取仪（ASE）萃取,固相萃取净化后,使用UPLC-ESI-MS/MS联用仪分析样品中11种PFCs.在6 min内就可快速稳定地将所选取的11种全氟化合物分离,且最低检测浓度为0.518—3.520 pg.g-1之间,这些化合物在土壤中的平均添加回收率在71.2%—119.2%之间.应用此方法测得宜兴市水稻土样品中所选取的PFCs含量为0.006—0.780 ng.g-1之间.