气质联用仪在鼠药、有机磷及氨基甲酸酯类农药中毒事件中的检测应用

目的在鼠药、有机磷及氨基甲酸酯类农药中毒事件中快速定性定量检测鼠药、有机磷及氨基甲酸酯类农药。方法气质联用法。结果18min内快速分离检测鼠药毒鼠强及甲胺磷、敌敌畏、氧化乐果、乐果、甲基对硫磷、马拉硫磷、克百威、抗芽威、甲奈威、对硫磷等有机磷及氨基甲酸酯类农药。结论气质联用法测定鼠药、有机磷及氨基甲酸酯类农药具有简便、快速、准确、灵敏等优点。该方法适用于中毒检样的检测。     

LC/MS/MS法同时测定食品中喹诺酮类药物

LC／MS／MS法同时测定食品中依诺沙星(Eno),氧氟沙星(Oflo),环丙沙星(Cip),达诺沙星(Dano),洛美沙星(Lome),恩氟沙星(Enro)和沙拉沙星(Sara)7种喹诺酮类药物。     

液相色谱串联质谱法定量检测血清中8种有机磷农药

目的建立了液相色谱串联质谱(LC-MS-MS)法测定血清中8种有机磷农药含量的方法。方法血清样品经乙酸乙酯液液萃取,以pH3.5的乙酸铵缓冲溶液,甲醇和水为流动相混合梯度洗脱,滤液经C185μm(2.1 mm#150mm柱)分离,经在线电喷雾离子源(ESI)正离子化后,采用多反应离子监测方式(MRM)选择离子对测定。结果目标化合物的线性范围为0～1000ng/ml,8种化合物相关系数均大于0.990,加标回收率为95%～129%,RSD<7.9%;日内日间相对标准偏差小于12%(n=6)。结论 LC-MS-MS方法高效、准确,特异性强,样品处理简单,可准确定量血清中有机磷农药。     

LC/MS/MS法对葡萄、葡萄酒及果汁中助壮素的测定

样品用水-甲醇(1:1)萃取,用氨水调pH 10, 用SDVB萃取柱净化。用LC/MS/MS法测定。定量下限1μg/kg。在葡萄、葡萄酒及果汁中添加5μg/kg和 50μg/kg助壮素,其添加回收率为84．5％-96．1％,标准偏差0．6％-6．4％。对市售的14个葡萄样品中5个检出助壮素(12．8μg/kg-199μg/kg),14个白葡萄酒     

食物中毒样品中的乌头碱的SPE—UFLC／MS／MS快速测定法

目的建立SPE．UFLC／MS／MS快速测定食物中毒事件中乌头碱、次乌头碱、中乌头碱的方法。方法各种食物样品及呕吐物经0．1mol／LHCl提取,SPE固相萃取小柱净化,经AgilentSBC182．1mm×50mm,1．8μm分离,在正离子模式下用串联质谱仪定性定量分析。结果食物样品及呕吐物中乌头碱、次乌头碱、中乌头碱的方法检出限为1—3μg／L,2个水平的加标回收率为79．8％～112．5％,相对标准偏差均小于9．4％。结论该方法测定各种食物样品及呕吐物中的乌头碱、次乌头碱、中乌头碱快速,准确,可靠,灵敏度高。     

有机磷农药及氨基甲酸酯类农药的GC和GC／MS谱库的建立

目的通过气相色谱法（GC）和气质联用法（GC／MS）实现对16种有机磷农药及8种氨基甲酸酯类农药的分析鉴定。方法通过分析农药标准选择合适的GC分离条件,从而建立各农药的色谱图库和质谱法（MS）库。结果各种农药在不同色谱条件均能达到较好的分离,分析时间在25min内,分析鉴定结果可信度高。结论3种检测方法配合使用,快速、准确,适用于多种农药残留及中毒分析。     

LC/MS/MS法分析啤酒及其原料中氟马菌素B1及B2

采用液相色谱-电喷雾电离串联质谱法（LC／MS／MS）测定啤酒及其原料中的氟马菌素B1（FB1）和氟马菌素B2（FB2）。样品经固相萃取柱（SAX）制备和净化，配有十八烷基二氧化硅柱的液相色谱分离，流动相由水和乙腈组成，流速0．2ml／min。用MS／MS电喷雾电离多元反应监测法（ESI-MRM）测定。     

食品中27种农药残留量的高效液相色谱-串联质谱测定法

目的建立以固相萃取/高效液相色谱-串联质谱(LC/MS)同时测定食品中27种农药残留量的方法。方法采用酸性乙腈匀浆提取。盐析离心后,过C18柱净化去脂,经LC/MS电喷雾电离(ESI)源,负离子多反应(MRM)模式检测,外标法定量。用乙腈-酸性水(pH=5)作为流动相,梯度洗脱,根据不同检测要求用液相色谱-串联质谱仪检测农药多残留组分。结果所有27种农药均在40 min内流出,农药标准的线性范围在0.05～10.0μg/ml,相关系数r均在0.99以上,低、高2种浓度加标回收率均在80.2%～96.2%之间,相对标准偏差均小于10%,方法最低检出限在0.001～0.040 mg/kg(S/N=3)。结论方法简单、快速、灵敏,适合于食品中有机磷、有机氯、拟除虫菊酯、氨基甲酸酯、除草剂等农药残留的测定,且准确度好,精密度高,适用于食品中27种农药同时分析。     

LC/MS法同时测定食品中9种甜味剂

用0.08mol/L磷酸盐缓冲液（pH7．0）-乙醇（1：1）直接提取食品中乙酰磺胺酸钾（AK）、三氯蔗糖（SUC）、糖精（SA）、环己基氨基磺酸盐（CYC）、阿斯巴甜（APM）、甘素（DU）、甘草酸（GA）、甜菊甙（STV）和甜菊苷A（REB）9种甜味剂，用C18柱净化。用5mmol／L乙酸二丁基铵（DBAA）和乙腈-水（8：2）为流动相，用LC／MS测定。在辣酱油等5种食品中添加0．01、0．05和0．20g／kg 9种甜味剂，其回收率为75．7％，109．2％。定量限AK、SA、CYC、APM和STV为0．001g／kg，SUC、DU、CA和REB为0．005g／kg。     

Analysis of Multiple Pesticides in Urban Storm Water Using Solid-Phase Extraction

An analytical method was developed using C₁₈ solid-phase extraction and gas chromatography—nitrogen phosphorus detection (GC-NPD) to determine the presence and quantity of 12 contemporary pesticides in storm water runoff from an urban environment. The method was validated, using deionized water and water collected from a local pond, for two concentration levels and four holding time regimes. The method was then utilized in a study examining nonpoint source (NPS) pollution in Wichita, KS. Accuracy and precision were demonstrated in each test for each analyte except diazinon, which degraded rapidly during holding times in aqueous solution. For all matrices, concentration levels, and holding times, mean recoveries for the remaining 11 pesticides ranged from 50% to 105% with percent relative standard deviations less than 25%. Received: 17 February 1999/Accepted: 7 April 1999     

HPLC-DAD-MS/MS法快速分析大黄中酚类成分

目的对中药大黄的有效成分进行快速分析。方法选用Waters XBridge C18柱为分析柱,流动相为乙腈与甲酸水梯度洗脱系统,流量为300μL/min;质谱条件选用电喷雾离子源(ESI),检测方式为负离子多级质谱全扫描,子离子采用动态排除法(DDS)。结果对总离子流图的主要色谱峰的多级碎片进行解析,结合对照品的裂解规律,综合紫外(UV)数据、保留时间及参考文献,共鉴别出了中药大黄中的14个化学成分。结论采用本方法可用于中药大黄的化学成分的快速分析与鉴定,HPLC-MS联用技术值得在中药药物分析与质量控制研究中应用和推广。     

GC/MS定性定量分析被化工原料污染河水中的β-蒎烯

目的 研究探讨GC／MS测定水中β—蒎烯的分析方法。方法 用二氯甲烷萃取各种水样中的β—蒎烯，运用GC／MS的Xcalibur分析软件的谱库检索功能，从NIST 98谱库中检索出被化工原料污染河水的成分是β—蒎烯。应用GC／MS快速准确定量测定了β—蒎烯在河水中的含量。结果 被化工原料污染河水中β—蒎烯含量为182．2μg／ml。结论 该方法简便、快速、灵敏度高、准确可靠。     

Profiling gangliosides from milk products and other biological membranes using LC/MS

Gangliosides are an important class of glycosphingolipids involved in numerous biological processes such as neuronal development, host–pathogen interactions and gastrointestinal health. Due to the highly heterogeneous nature and relatively low abundance of gangliosides, characterization of gangliosides in biological membranes is challenging. Existing methods for ganglioside analysis are quite time consuming and require expensive high resolution mass spectrometers. A rapid method combining reversed phase chromatography and mass spectrometry was developed using a triple-quadrupole mass spectrometer operating in multiple reaction monitoring mode. The ganglioside species were separated with a Poroshell 120 EC-C18 column and analysed under the negative ion mode. This method allows a sensitive, specific, and quantitative assay for profiling gangliosides. The method is developed for analysis of gangliosides in the milk fat globule membrane of whole milk and applied to other biological membranes. Application includes the cellular membrane of prostate cancer cells. In summary, the method allows various biological membranes to be screened for over 600 gangliosides from 12 classes (GM1, GM2, GM3, GM4, GD1, GD2, GD3, GD4, GT1, GT2, GT3, and GT4) in less than three hours. In summary, expressed as % of relative amounts: 1.5% GM3, 80.2% GD3, 14.4% GT3, 1.5% GM1, 2.4% GD1 were observed in whole milk; 2.5% GD1, 88.2% GD3, 2.5% GM1, 2.2% GM3, 0.2% GT2, 4.2% GT3 were observed in buttermilk and 10.6% GD1, 55.6% GD3, 1.6% GM1, 12.2% GM3, 19.2% GT3, 0.9% GT4 were observed in colostrum.     

Organochlorine Pesticides and Enantiomers of Chiral Pesticides in Arctic Ocean Water

In the summers of 1993 and 1994, seawater samples from the surface layer (40–60 m) were collected to determine the spatial distribution of organochlorine pesticides on expeditions that crossed the Arctic Ocean from the Bering and Chukchi seas to the North Pole, to a station north of Spitsbergen, and then south into the Greenland Sea. Spatial differences in concentration were found that varied with the pesticide. Heptachlor exo-epoxide (a metabolite of heptachlor) and α-hexachlorocyclohexane (α-HCH) increased from the Chukchi Sea to the pole, and then decreased toward Spitsbergen and Greenland Sea. Chlorinated bornanes (toxaphene) followed a similar trend, but levels were also high near Spitsbergen and in the Greenland Sea. A reverse trend was found for endosulfan, with lower concentrations in the ice-covered regions. Little variation was seen in chlordane concentrations, although the ratio of trans-/cis-chlordane decreased at high latitudes. Several of these pesticides are chiral: α-HCH, cis- and trans-chlordane, and heptachlor exo-epoxide. Enantioselective degradation of (−)α-HCH was found in the Bering and Chukchi seas, whereas the (+) enantiomer was depleted in the Arctic Ocean and Greenland Sea. Enrichment of (+) heptachlor exo-epoxide was found in all regions. Trans- and cis-chlordane were nearly racemic. Received: 4 October 1997/Accepted: 19 February 1998     

Simultaneous determination of 42 organic chemicals in bottled water by combining C18 extraction disk with GC-MS and LC/MS/MS technique

A method for the determination of 42 hazard residues required by ‘Japan Positive List System’ in bottled water was described. Hazard compounds in bottled water were extracted with a solid phase extraction step using C18 disks. Determination was carried out by gas chromatography/mass spectrometry (GC/MS) and liquid chromatography-tandem mass spectrometry (LC/MS/MS). The disk extraction has high throughput which is well adapted to isolate and enrich these compounds from large volumes of water. For the water sample spiked at three concentration levels (LOQ, 4 times LOQ and 8 times LOQ), the recoveries of all analytes ranged between 65% and 120% with a relative standard deviation < 24% (n=8).     

氨基甲酸酯类农药的微色谱快速检测法

目的利用毛细管效应建立制备微色谱柱检测器以快速检测氨基甲酸酯类农药。方法在薄层色谱原理的基础上,通过将吸着剂固定于细加热丝上,利用毛细管效应制备微色谱柱检测器,对氨基甲酸酯类农药作出快速的定性分析。结果该方法可以对氨基甲酸酯类农药作出快速的定性分析,且最低检出量可达到50μg。结论该法操作简便,高效,重现性好,且试剂用量少,是批量氨基甲酸酯类农药样品定性检测和突发农药中毒事件现场快速筛选的一种新方法。     

Organophosphorous Pesticides in Surface Water of Iran

This research aims to evaluate the presence and distribution of pesticides in Babolrood River of Mazandaran Province in Iran. Mean diazinon levels in surface water ranged from 77.6 to 101.6 μg L⁻¹ with maximum level of 768.9 μg L⁻¹ and mean malathion levels ranged from 55.7 to 75.9 μg L⁻¹ with maximum level of 506.6 μg L⁻¹. The residues of malathion and diazinon pesticides in all of the stations, 2 weeks after spraying, were more than allowed limits.     

七种有机磷农药残留量的快速毛细柱气相色谱分析

本文报道了应用毛细柱气相色谱同时对七种有机磷农药残留量快速的分析方法。本方法使用了一支25m×0.2mm OV—101石英毛细柱及FPD检测器,以分流进样方式,一阶程序升温(150℃→(20℃/分)210℃,保持8分钟),在11分钟之内可完成气相色谱分析。七个色谱峰完全分离。分流比在20～140范围内,线性检验结果良好。最低检测限为2.3×10~(-10)～5.4×10_(-10)g,平均相对标准偏差小于10％。三个水平的平均回收率分别为75.3％、82.2％和87.9％。样品予处理采用氯仿—甲醇(9:1)混合液为提取剂,使用一只长颈漏斗将提取和净化步骤一次完成。     

一起水污染事件的吹扫捕集-气相色谱-质谱的分析结果

2010年7月29日,昆山市疾病预防控制中心接某乡镇打工楼的某公司职工反映,该宿舍楼自来水有异味,部分职工饮用后出现恶心反应,本中心接报后立即赶赴现场调查处理。该宿舍楼二期工程(5、6、7号楼)刚于本月初竣工,某公司职工90人于2周前入住,现场调查发现,(5、6、7号楼)各楼层自来水末梢水均有油漆味,刚开启时尤甚,放水一段时间后气味减轻,而一期工程的宿舍(1、2、3、4号楼)、食堂等处自来水未发现异味。     

样品中有机磷与氨基甲酸酯类农药快速检测方法的建立

目的建立现场快速筛选区分有机磷农药和氨基甲酸酯类农药的方法。方法在薄层色谱原理基础上,利用毛细管效应制备微色谱柱检测仪,检测2类农药。结果该方法可以对有机磷农药和氨基甲酸酯类农药作出快速的定性分析,且最低检出量可达到10μg。结论该法操作简便,高效,重现性好,且试剂用量少,是批量农药样品定性检测和突发农药中毒事件现场快速筛选的一种新方法。