超高效液相-质谱联用法测定化妆品中9种禁用激素

建立化妆品中非法添加的9种糖皮质激素的快速测定方法。采用超高效液相色谱-串联质谱法(UPLC-MS/MS),以ACQUITY UPLC~BEN C18色谱柱(50 mm×2.1 mm,1.7μm),流动相采用甲醇-水,电喷雾电离(ESI)联合相关信息扫描(IDA)与增强离子扫描(EPI)的扫描方式,对化妆品中非法添加的9种糖皮质激素成分进行快速定性分析,检测限低于0.4μg/m L。     

超高效液相色谱-串联质谱法测定菠菜、苹果及大豆中二硝基苯胺类除草剂残留量

以菠菜、苹果和大豆为代表性分析物,建立了超高效液相色谱 串联质谱法（UPLC-MS/MS）检测蔬菜、水果及粮谷等植物源性食品中8种二硝基苯胺类除草剂（氟乐灵、二甲戊乐灵、仲丁灵、异乐灵、磺乐灵、氨基乙氟灵、氨磺乐灵和氨基丙氟灵）的残留量。采用电喷雾电离,正离子扫描,多反应监测（MRM）模式检测,并使用外标法定量。结果表明：8种二硝基苯胺类除草剂的测定低限均为10 μg/kg;在添加水平10~200 μg/kg范围内,加标回收率为70.0%～120%,相对标准偏差为0.56%～23.0%。该方法灵敏、有效,适用于蔬菜、水果和粮谷等植物源性食品中二硝基苯胺类除草剂多残留的测定。     

UPLC-MS/MS法同时检测饲料中5种氨基糖苷类抗生素

建立了UPLC-MS/MS检测饲料中5种氨基糖苷类抗生素(链霉素、丁胺卡那霉素、安普霉素、庆大霉素、新霉素)的分析方法,样品用高氯酸溶液酸解及沉淀蛋白质,经MCX固相萃取净化、富集后,以10 mmol/L乙酸胺溶液(含0.1%甲酸)-乙腈作为流动相进行梯度洗脱,采用多反应监测(MRM)模式进行定性和定量分析。5种氨基糖苷类在10~500 ug/L的范围内线性关系良好(r≥0.9989)在10、50、100μg/kg添加水平下的回收率为74%~93%,RSD(n=6)为3.1%~8.1%,定量限(LOQ)为≤5μg/kg,该方法精密度好,灵敏度高,能简便、快速、准确地测定饲料中的5种氨基糖苷类抗生素。     

UPLC-MS/MS 法检测祛痘类化妆品中盐酸特比萘芬含量

采用超高效液相色谱-串联质谱法(UPLC-MS/MS)建立了祛痘类化妆品中盐酸特比萘芬的检测方法。待测样品以甲醇为提取溶剂经超声提取,上清液经微孔滤膜过滤后测定。以10 mmol/L乙酸铵水溶液-乙腈为流动相,BEH-C18色谱柱分离,采用多反应离子监测(MRM)模式进行定性定量分析。所建方法中,待测组分检出限为0.02 mg/kg,定量限为0.05 mg/kg,在低、中、高3个添加水平范围内平均回收率为89.0%~117.7%,相对标准偏差为1.1%~4.7%。用于80批祛痘类化妆品样品检测,其中1批检出盐酸特比萘芬。     

UPLC-MS/MS法同时测定减肥食品中55种非法添加物

目的 建立超高效液相色谱-串联质谱同时测定减肥类食品中55种非法添加物的分析方法。方法 样品经甲醇超声提取后,采用Agilent Eclipse Plus C₁₈ RRHD色谱柱(2.1 mm×100 mm,1.8μm)分离,以乙腈-0.1%甲酸为流动相进行梯度洗脱。在正负离子扫描条件下,采用动态多反应监测模式监测。结果 55种非法添加药物在相应的线性范围内均呈现良好线性关系,相关系数大于0.995,平均回收率75.2%～121.6%,相对标准偏差<12%,各化学药物的检测限在0.02～1.25μg/g。应用该方法对50批样品进行了检测,其中有38批次样品检出托拉塞米、大黄素、西布曲明、N-单去甲基西布曲明、N,N-双去甲基西布曲明、比沙可啶、麻黄碱、甲基麻黄碱、氢氯噻嗪、氟西汀等非法添加物。结论 该方法简单、快速、灵敏、准确、高效,兼具定性定量检测的优点,可用于食品中减肥类化学药物的高通量检测。     

Novel approach to fast determination of multiple pesticide residues using ultra-performance liquid chromatography-tandem mass spectrometry (UPLC-MS/MS)

A rapid, high-throughput method employing ultra-performance liquid chromatography with tandem quadrupole mass spectrometry (UPLC-MS/MS) was developed and optimized for simultaneous quantification and confirmation of 64 pesticide residues and their toxic metabolites in fruit extracts prepared by a buffered QuEChERS procedure. The total time required for UPLC-MS/MS analysis was 8 min plus 2 min for re-equilibration to the initial UPLC conditions. Performance characteristics were determined for apple extracts spiked at 10 µg kg^?1. The repeatability of measurements expressed as relative standard deviations was in the range 1.5–13% at this level for most analytes. Thanks to very low limits of quantification (<10 µg kg^?1for the majority of pesticides), an optimized method allows for the reliable control of not only common maximum residue limits (MRLs) set by European Union regulation for various pesticides/fruit combinations, but also of a uniform MRL of 10 µg kg^?1endorsed for baby food.     

Simultaneous determination of three pesticides and their metabolites in unprocessed foods using ultraperformance liquid chromatography-tandem mass spectrometry

We have developed a rapid, multi-compound analytical method for measuring residues of the pesticides thiamethoxam and its metabolite, clothianidin; fipronil and its three metabolites, fipronil sulfone, fipronil sulfide, and fipronil desulfinyl; and pyraclostrobin in unprocessed foods (rice, corn, cucumbers, tomatoes, apples, and bananas) by ultra-performance liquid chromatography coupled to tandem mass spectrometry. Acetonitrile was used as the extraction solvent, and an octadecylsilane-dispersive SPE was used to clean up the analytes, which were then separated through a UPLC HSS T3 column connected to a tandem mass spectrometer via an electrospray ionisation source. The linearity of this method for the target analytes was excellent (R² ≥0.990) in the concentration range of 5–1000 μg kg^–1. The average recoveries of the seven compounds at concentrations of 10, 100, and 1000 μg kg^–1 from six spiked matrix samples ranged from 73.6 to 110.6%, all with RSD values of ≤19.7%. The limit of quantification was 10 μg kg^–1. The method validated the effectiveness of the method for routine monitoring the residue of these pesticides and their metabolites in foods.     

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.     

UPLC-MS/MS检测鸡蛋中22种喹诺酮类药物残留方法的研究

应用超高效液相色谱串联质谱建立鸡蛋中加雷沙星、曲伐沙星、莫西沙星、奥比沙星、吉米沙星、加替沙星、培氟沙星和环丙沙星等22种喹诺酮类药物残留检测方法。样品经过2%甲酸乙腈提取、正己烷分步去脂,Oasis HLB柱净化后,经Acquity UPLC BEH Shield RP18(100 mm×2.1 mm,1.7μm)分离,以甲醇和0.1%甲酸水溶液为流动相进行梯度洗脱,双通道MRM信号采集模式,22种喹诺酮类药物能在11 min完好分离,方法的最低定量限均低于1.0μg/kg,在2.0~100.0μg/L浓度范围内,22种喹诺酮类药物线性良好,相关系数均在0.99以上;通过2、10、20 g/kg三个浓度的加标回收实验表明,回收率为60.1%~96.2%,RSD%值为1.44%~11.1%。该方法相比现有国标检测药物种类多,新型药物多,对更全面筛查和确证鸡蛋中喹诺酮类药物残留,防范非法添加造成安全隐患具有一定的参考价值。     

低聚合度壳寡糖制备及其组分的色谱行为分析

利用壳聚糖酶水解壳聚糖,再通过乙醇沉淀法制备低聚合度(Dp＜6)的壳寡糖.利用Shodex NH2P-50 4E色谱柱,以乙腈-氨水为流动相梯度洗脱,建立了一种分离度好、灵敏度高的壳寡糖HPLC分析方法;利用UPLC-MS定性鉴定壳寡糖中N-乙酰化的组分.研究还探讨了壳寡糖组分的色谱行为,发现壳寡糖的N-乙酰化是导致壳寡糖不按照聚合度大小进行色谱分离的主要原因,为壳寡糖质量分析、组分分离提供了依据.