超高效液相色谱-串联质谱法测定食品中黄曲霉毒素B1和M1的方法研究

应用超高效液相色谱-串联质谱联用技术（UPLC-MS/MS）,在多反应离子检测（MRM）方式下对食品中的黄曲霉毒素B1（AFB1）和M1（AFM1）污染量进行检测.样品经乙腈-水混合试剂提取,中性氧化铝柱净化,经Agilem ZORBAX Eclipse plus C18色谱柱（100 mm×4.6 mm,1.8 μm）,以甲醇和10 mmol/L NH4Ac溶液（含0.1％的甲酸）为流动相洗脱分离,以MRM方式进行定量分析.AFB1和AFM1分别在0.12～6.12 μg/L和0.11～2.28 μg/L质量浓度范围内线性关系良好,相对标准偏差（RSD）＜5％,加标回收率为81.3％～97.2％.该方法具有低成本、准确、快速、简便、灵敏度高等优点,可满足我国对AFB1和AFM1检测限要求.     

QuEChERS萃取-UPLC-MS/MS测定花生酱中黄曲霉毒素B1方法的研究

建立了QuEChERS萃取-UPLC-MS/MS测定花生酱中黄曲霉毒素B1的快速检测方法。样品首先经过1%甲酸-乙腈溶液提取,提取液采用QuEChERS净化试剂(250mg MgSO4+100mg HC-C18+50mg PSA)净化后上机,UPLC-MS/MS正离子源多反应模式检测,外标法定量。黄曲霉毒素B1在1.0~5.0ng/mL范围内呈良好线性关系,相关系数(R^2)>0.999,4个水平的添加目标分析物黄曲霉毒素B1的回收率在81.7%~93.5%范围内,相对标准偏差(RSD)为2.4%~5.6%,检出限为0.03μg/kg;该试验方法具有简单、高效、经济、准确、回收率高、精密度好的优点,适用于花生酱样品中黄曲霉毒素B1的快速检测。     

酶联免疫吸附结合免疫亲和柱－高效液相色谱法检测大米中黄曲霉毒素B1的研究

对大米中两种检测黄曲霉毒素B1方法的结合使用进行了研究,即采用酶联免疫吸附法对大米中黄曲霉毒素B1进行初筛,对可疑样品采用免疫亲和柱-高效液相色谱法进行验证。样品经甲醇水提取、免疫亲和柱净化、高效液相色谱分离、碘柱后衍生、荧光检测器测定。结果表明,黄曲霉毒素B1线性关系良好,相关系数为0.9999,检出限为0.50μg/kg,回收率为89.4%~95.2%,RSD值为1.88%~3.05%。两种方法的结合应用,适用于较大批量样品的检测。     

Aflatoxin M1 in raw,UHT milk and dairy products in Sicily (Italy)

A survey on 73 milk samples from different animal breeds and 24 dairy products samples from Sicily, Italy, was carried out for the presence of aflatoxin M₁ (AFM1) by LC-fluorescence detection after immunoaffinity cleanup. AFM1 was detected in 48% and 42% of the milk and dairy samples at concentration ranges between <5.0–16.0 and <5.0–18.0 ng L^?1, respectively. Within the raw milk samples, 92% had an AFM1 content below 5.0 ng L^?1, in 7% of the cases it was in the range 5.0–10.0 ng L^?1 and 1% was contaminated between 10.0 and 20.0 ng L^?1. For the dairy products, ultra-high-temperature treated (UHT) milk, milk cream and cheese, the incidence was 42%, of which 83% contained less than 5.0 ng L^?1 and 17% contained 10.0–20.0 ng L^?1 AFM1. The levels of contamination found justify continuous monitoring for public health and to reduce consumer exposure.     

LC-MS/MS法测定人血浆中曲司氯铵的浓度

目的建立测定人血浆中曲司氯铵浓度的LC—MS／MS方法。方法血浆样品经液-液提取后,以甲醇（含0．1％乙酸）：水（含0．1％乙酸＋2．5mmol／L酸铵）（80：20）为流动相,使用Agilent1100VL型离子阱质谱仪,电喷雾离子源正离子模式,采用多反应离子监测方式测定曲司氯铵（MRM,m／z392→164＋182）。结果血浆中曲司氯铵线性范围为0．1～10．0ng／mL,定量下限为0．1ng／mL,准确度85％～115％,日内、日间精密度（RSD）&#177;15％。结论该方法准确,专属性强,可用于曲司氯铵药动学研究。     

Reduction of Aflatoxin M1 from Artificially Contaminated Milk Using Ultrafiltration and Diafiltration

The effect of ultrafiltration-diafiltration (UF-DF) on removal of aflatoxin M₁ (AFM₁) from raw whole, homogenized and acidified milk was studied. Milk was artificially augmented with concentrations of AFM₁ varying from 0.5 to 3.5 μg/L. The removal of AFM₁ was influenced (p<0.05) by the initial concentration and the homogenization process. Homogenization and acidification decreased the removal of AFM, from milk. The UF-DF process did not result in concentrates within permissible residual levels at any concentration studied. However, reconstituted retentates had residual levels of AFM₁ < 0.5 μg/L resulting from milk originally containing up to 2 μg/L.     

液相色谱-串联质谱法测定豆类中左旋多巴

文章建立一种豆类中左旋多巴的液相色谱-串联质谱测定方法。样品经0.3 mol/L乙酸水溶液超声提取,Agilent Proshell 120 SB-C18(2.1 mm×150 mm,2.7μm)色谱柱分离,以0.1%甲酸水-甲醇为流动相进行梯度洗脱,多反应监测(MRM),内标法定量。结果表明,左旋多巴在0.1~5.0 mg/L范围内线性关系良好,相关系数为0.9994,检出限为1.5 mg/kg,定量限为5.2 mg/kg,方法的平均加标回收率为96.9%~105.5%,日内精密度和日间精密度均小于4%,具有操作简单、灵敏度高、准确度高、重现性好等特点,能够很好满足豆类中左旋多巴含量的检测需要。     

比对实验中黄曲霉毒素B1的检验与分析

本文综合国标法,色谱法及试剂盒法三种方法进行修正,把1：1的甲醇水改为7：3的甲醇水直接加进样品中,删除国标法及试剂盒自带方法中采用石油醚转移步骤,把手动振摇、蒸发等步骤改为漩涡振荡及离心方法,改良了样品的提取方法,操作方便,减少交叉污染,使结果更稳定。     

LC-MS/MS法测定人血浆中曲司氯铵的浓度

目的建立测定人血浆中曲司氯铵浓度的LC-MS/MS方法。方法血浆样品经液-液提取后,以甲醇(含0.1%乙酸):水(含0.1%乙酸+2.5mmol/L甲酸铵)(80:20)为流动相,使用Agilent1100VL型离子阱质谱仪,电喷雾离子源正离子模式,采用多反应离子监测方式测定曲司氯铵(MRM,m/z392→164+182)。结果血浆中曲司氯铵线性范围为0.1～10.0ng/mL,定量下限为0.1ng/mL,准确度85%～115%,日内、日间精密度(RSD)±15%。结论该方法准确,专属性强,可用于曲司氯铵药动学研究。     

卷烟主流烟气中挥发性醛酮的LC-MS/MS分析

采用2,4-二硝基苯肼衍生-LC-MS/MS法测定了32种卷烟样品主流烟气中的甲醛、乙醛、丙烯醛、丙酮、丙醛、巴豆醛、甲基丙烯醛、2-丁酮、丁醛、苯甲醛、戊醛、己醛.结果表明:①方法的检测限为0.1～0.5 ng/mL,回收率在91.6%～100.3%之间,相对标准偏差为3.28%～7.86%;②卷烟样品主流烟气的挥发性醛酮成分中主要为乙醛和丙酮,苯甲醛、已醛含量较小;③与进口烟相比,国产烤烟型卷烟主流烟气中的挥发性醛酮含量相对较高,混合型卷烟的相对较低;④不管是烤烟型还是混合型,焦油量高的卷烟主流烟气中的挥发性醛酮含量均相对较高.     

LC-MS/MS测定鞋材中的全氟辛烷磺酸盐

建立了纺织品和皮革样品中全氟辛烷磺酸盐(PFOS)的提取方法,样品用甲醇或乙腈超声提取,提取液经C18柱净化,去除基质干扰后用液相色谱-质谱/质谱联用法(LC-MS/MS)检测,标准曲线线性良好,相关系数r=0.9996,灵敏度高,若是刮表层的检出限为0.4μg/m2,若是称重的检出限为0.02 mg/kg,回收率达78%～89%.     

高效液相色谱-串联质谱法同时测定花生制品中的黄曲霉毒素B1、B2、G1、G2

采用高效液相色谱-串联质谱建立了高效液相色谱-串联质谱法同时测定花生制品中4种黄曲霉毒素(B1、B2、G1、G2)的方法.结果表明,在ESI正离子模式下,高效液相色谱-串联质谱法的最低检出限为0.2μg/kg,定量限为0.6 μg/kg;标准工作液在0.5～50.0μg/kg的范围内线性良好,相关系数达到0.9990.     

液相色谱串联质谱法测定食品中红曲色素

采用液相色谱串联质谱法测定了食品中红曲红胺、红曲红素、红曲素、红曲黄素的含量,并选择离子检测进行阳性确证。液体试样用水超声提取,离心定容后,固体和半固体样品采用水溶解定容,提取液再经固相萃取柱净化,样液经洗脱定容后,供液相色谱-质谱/质谱仪测定和确证,外标法定量。该方法的最低检出限、线性范围和方法回收率分别为:1.0 mg/kg、1.0～100.0 mg/kg和89.3%～94.3%。     

液相色谱-串联质谱法测定葡萄酒中赭曲霉毒素A

以赭曲霉毒素B为内标物,建立了应用固相萃取-液相色谱-串联质谱法(SPE-LC-MS/MS)对葡萄酒中赭曲霉毒素A残留量测定的方法。葡萄酒样品经过调节pH值至7.0和C18固相萃取净化的前处理过程后,采用液相色谱-串联质谱法进行测定(正离子方式,多反应监测模式)。方法定量限(LOQ)为2.0g/L。内标法定量计算,在0~10g/L质量浓度范围内线性相关系数0.998。在葡萄酒中分别进行2.0g/L、4.0g/L和8.0g/L三个添加水平的测试,该检测方法回收率范围97.6%~109.7%,相对标准偏差(RSD)3.0%~4.6%。方法简便、快速、准确,可用于葡萄酒中赭曲霉毒素A的定量测定。     

高效液相色谱串联质谱法分析烟草中15种农药残留

为检测烟草中的“吡蚜酮”等农药残留,建立了乙腈提取、分散固相萃取净化和高效液相色谱-质谱联用(LC-MS/MS)快速分析烟草中15种农药残留的方法.结果表明:15种农药在0.10,0.25和0.50 μg/g 3个加标水平的回收率为70.43% ～ 117.81%,相对标准偏差(RSD)为1.16%-13.89%,检出限为0.004～0.030 μg/g.该方法适合于批量烟草样品中多种农药残留的快速分析.     

Determination of androstenone levels in porcine plasma by LC-MS/MS

Androstenone (5α-androst-16-en-3-one) is a major component in boar taint. Here, a liquid chromatography-tandem mass spectrometry method was developed to analyse androstenone in porcine plasma to facilitate studies of its transport from pig testes to adipose tissues. The method used androstanone (5α-andro-stan-3-one) as internal standard, Oasis® MCX solid-phase extraction, C18 reversed-phase column, and API 5000 Triple Quadrupole mass spectrometry with positive electrospray ionisation interface operating in the multiple reaction monitoring mode. Incubation of the plasma samples with β-glucuronidase/arylsulfatase revealed an increase in androstenone yield indicating the presence of a conjugated form of its 3-enol isomer. With this method the limit of detection (LOD) was 1.0 ng and the limit of quantification (LOQ) was 3.3 ng per mL of plasma. In conclusion, the presented method is sensitive and reproducible and thus suitable for accurate quantification of androstenone levels in a small volume of porcine plasma.     

Short communication: Occurrence of aflatoxin M1 in the Manchego cheese supply chain

The importance of ewe milk lies in the production of high quality cheeses, such as Manchego cheese with a Protected Designation of Origin, whose safety must be guaranteed. In a 2-yr study, 407 bulk tank milk samples from farms and 82 silo milk and curd samples from cheese factories were collected from southeast Spain and tested for aflatoxin M1 (AFM1) using 2 commercial ELISA tests. Of these, 99.3% of the bulk tank samples had AFM1 levels below the European Union (EU) legal limit for milk (50 ng/kg), and well below the limit adopted by the Codex Alimentarius (500 ng/kg). Moreover, 98.8% of the silo milk and curd samples from cheese factories had AFM1 levels below the EU limit for milk. When considering median AFM1 concentrations, an average 4-fold increase was found in the final curd in relation to the corresponding silo milk. Control of AFM1 in Manchega ewe milk would enhance dairy product safety by the possible detection of faults in the manufacture of Manchego cheese.     

Multiresidue automated turbulent flow online LC-MS/MS method for the determination of antibiotics in milk

A fast and reliable multiresidue method is reported for the identification and quantification of 36 different compounds from seven different classes of antibiotics (aminoglycosides, sulfonamides, macrolides, quinolones, tetracyclines, lincosamides and trimethoprim) in milk. Automated online sample cleanup was applied using turbulent flow chromatography (Transcend TLX system), directly coupled to a mass spectrometer (MS/MS) for sensitive and specific detection. The method involved a simple extraction/protein precipitation using acetonitrile, followed by centrifugation and filtration. After this preliminary step, the extract was injected into the TLX-ESI-MS/MS using optimised turbulent flow and liquid chromatography (LC) conditions. Single-laboratory validation of the method was carried out according to the Directive 2002/657/EC, clearly demonstrating the suitability of this method for quantitative determination of this wide range of antibiotics in milk. A small survey, which covered milk samples of different origin and varied fat content, demonstrated the robustness of this method and its suitability for enforcement purposes.     

LC-MS/MS测定肠衣中7种大环内酯类抗生素残留量

建立猪肠衣中螺旋霉素、替米考星、竹桃霉素、泰乐菌素、红霉素、罗红霉素、交沙霉素等7种大环内酯类抗生素残留量的液相色谱-串联质谱测定方法(LC/MS/MS).样品用甲醇提取,Oasis( HLB)固相萃取柱净化,液相色谱-串联质谱测定,外标峰面积法定量.方法的回收率范围为70.9 ％～98.4％;相对标准偏差5.8 ％～17.8％,7种大环内酯类抗生素的检出限均为20 μg/kg.     

液相色谱串联质谱法测定纸制品中PFOS

采用ASE-300快速溶剂取革仪提取样品中全氟辛烷磺酰基化合物(PFOS),经浓缩、净化、过膜、定容后,用液相色谱串连质谱法测定,外标法定量.采用选择离子检测进行阳性确证,提出了纸制品中PFOs的检测方法.本方法的最低检出限、线性范围和方法回收率分别为:0.10mg/kg、0.10～10.0mg/kg和71.0%～103.0%.