Finding of pesticides in fashionable fruit juices by LC–MS/MS and GC–MS/MS

Products labelled as containing extracts from two mushrooms (cordyceps plus reishi) and the juices from açaí, goji, mangosteen, noni, pomegranate, and sea buckthorn have been analysed for 174 different pesticides, using the validated QuEChERS method for sample preparation and electrospray LC–MS/MS in the positive ion mode for analysis. Pesticides were found in 10 of the 21 samples analysed. Most pesticides found were below the tolerance levels (1–6 μg/g, depending on the pesticide), but some were not. This included boscalid, dimethomorph, iprovalicarb, pyridaben, pyrimethanil, and imazalil, for which there is no tolerance reported or zero tolerance in any fruit. However, genuine açaí that was harvested in the state of Pará and lyophilised in Rio de Janeiro had no detectable pesticides, when analysed by both LC–MS/MS and GC–MS/MS, which can detect 213 more pesticides and industrial chemicals. Likewise no pesticides were found in one sample each of cordyceps plus reishi, sea buckthorn and noni.     

LC/MS/MS法分析食品中的三聚氰胺

奶粉类食品前处理1.所需试剂及耗材1%三氯乙酸溶液,0.1mol/L盐酸溶液,5%氨水-甲醇溶液,以及OasisMCX固相萃取柱(60mg/3mL,或相当者),使用前分别用3mL甲醇、3mL0.1mol/L盐酸溶液对固相萃取柱进行预处理,并保持柱体的湿润。     

HPLC-DAD和LC/MS/MS测定豆奶中三聚氰胺

目的:建立二极管阵列高效液相色谱仪和三重四级杆液质联用仪对豆奶中三聚氰胺的测定方法。方法:采用三氯乙酸和乙腈为提取剂、蛋白质为沉淀剂,提取液过净化柱纯化。结果:三重四级杆液质联用法对三聚氰胺的检出限为0.001 5 mg/kg,标准曲线在0.01~0.5μg/mL范围内,R~2为0.999 8,线性良好,再回收率为85%~89%,适用于检测低浓度的样品;二极管阵列高效液相色谱法检出限为0.024 mg/kg,标准曲线在0.5~100μg/mL范围内,R~2为0.999 9,线性良好,回收率为83%~91%,可以快速地对高浓度样品进行筛查。结论:以上两种检测方法结合使用,可检测0.01~100 mg/kg的三聚氰胺含量,极大地拓宽了检测范围。     

基于UPLC/Q-TOF MS/MS的花生油成分分析

采用超高效液相色谱-串联四级杆飞行时间质谱(UPLC/Q-TOF MS/MS)联用仪对花生油甲醇提取液分离检测,分析花生油成分,并通过二级质谱图和标准品确定物质。结果表明:正离子模式下检出86种化合物,鉴定30种物质,其中芥酸、棕榈酰胺、硬酯酰胺、油酸酰胺、11Z-二十二碳二烯酸为已知的花生油成分,亚油酰乙醇胺、亚油酰胺、鞘氨醇、N-油酰乙醇胺、十八碳四烯酸、顺-4-癸二酸等26种物质均为首次被检出;在负离子模式下,共检出27种化合物,鉴定15种物质,其中包括花生油中常见的7种脂肪酸,首次检出(Z)-13-氧-9-十八烯酸、蓖麻油酸、烯油酸、13-羟基十八酸和2(R)-羟基海藻酸5种脂肪酸和其他3种物质。     

基于UPLC/Q-TOF MS/MS的芝麻油成分分析

为发现芝麻油中新成分,通过UPLC/Q-TOF MS/MS对4种芝麻油甲醇提取液进行检测分析。结果表明：4种芝麻油中共发现143种共同物质,其中正离子模式71种,负离子模式72种。共同物质中鉴定出77种物质,其余66种为未鉴定成分;77种鉴定成分中包括脂肪酸及衍生物(8种)、芝麻素、芝麻林素、硬脂酰胺等12种已知成分,其余65种为新发现成分;新发现成分包括油酸酰胺、棕榈酰胺、亚油酰胺、芥酸酰胺、8-甲基-N-香草基壬酰胺、辣椒酰胺、N-硬脂酰丙氨酸等17种脂肪酸酰胺,十六碳烯酸、十八碳烯酸等22种脂肪酸及衍生物,5-脱氧基维醇、天孢菌素等5种类黄酮,马泰树脂醇、银杏酸等21种其他成分。芝麻油中含有大量新成分和未知成分,富含的脂肪酸、脂肪酸酰胺、类黄酮、木脂素等物质可解释其独特生理功能。     

MS发布高速印花机

近日，意大利MS公司发布了高速数码印花机LaRio。该机生产速度可达每分钟75m，幅宽1．8m，可完成8000m＾2／h印花业务，每天产能接近20万m＾2，堪比传统圆网印花机。该机目前已有一台在意大利投入实际生产使用。该机采用非接触的喷墨打印技术，实现对于墨水（染料）的精微控制，无须制版，印花得色率高，     

DLLME-LC/MS/MS法快速检测食用油中黄曲霉毒素

试验建立了分散液相微萃取技术和高效液相色谱-串联质谱联用快速分析食用油中5种黄曲霉毒素的新方法。食用油样品先用正己烷溶解分散,再用一定比例的乙腈和水萃取,振荡漩涡离心后LC-MS/MS测定。试验对影响萃取效果的因素进行了优化,在优化试验条件下,方法的线性范围为0.06~10μg/kg,检出限为0.02~0.03μg/kg,相关系数为0.993 3~0.999 0,样品加标回收率为70.2%~86.8%,相对标准偏差为2.4%~7.3%。该方法已成功应用于食用油中黄曲霉毒素的分析测定。     

三聚氰胺检测五LC/MS/MS法分析食品中的三聚氰胺

奶粉类食品前处理 1.所需试剂及耗材 1%三氯乙酸溶液,0.1mol/L盐酸溶液,5%氨水-甲醇溶液,以及Oasis MCX固相萃取柱(60mg/3mL,或相当者),使用前分别用3mL甲醇、3mL0.1mol/L盐酸溶液对固相萃取柱进行预处理,并保持柱体的湿润.     

塑料包装材料中邻苯二甲酸酯的LC/MS/MS测定方法研究

建立了LC/MS/MS测定塑料包装材料中邻苯二甲酸酯含量的分析方法.将塑料包装材料粉碎后索氏提取,经LC/MS/MS分析在50μg/L～400μg/L范围内呈现良好的线性关系(R2＞0.9985),方法检测限小于35μg,/kg;在50μg/kg、200μ g/kg、400μg/kg三个样品加标水平,PAEs的回收率在91.42％～99.90％之间;方法精密度实验的相对准偏差在5％之内.结果表明该方法准确可靠,精密度较高.     

ASE-GPC-LC/MS/MS联用检测贝类样品中扑草净的残留

建立了ASE(快速溶剂提取)、GPC(凝胶渗透色谱仪)、(液相色谱-质谱联用)LC/MS/MS法检测贝类样品中扑草净残留量的分析方法。本实验采用乙腈经ASE上机提取,凝胶渗透色谱仪净化,最后通过液相色谱-串联质谱进行定量检测。实验结果表明:扑草净在线性范围为0.25~40μg/kg时,线性关系良好(R2=0.9999),回收率为90.0%~105.4%,相对标准偏差2.9%~5.3%。     

蔬菜中噻虫嗪农药残留LC/MS/MS测定

利用液相色谱-串联质谱法(LC/MS/MS)建立了蔬菜中噻虫嗪农药测定的方法。方法试样中噻虫嗪农药残留在超声波振荡条件下用乙腈提取,经石墨化炭黑(Carb)和N-丙基乙二胺(PSA)粉末净化,经液相色谱质谱联用仪检。噻虫嗪农药残留的色谱图分离效果良好,在0.5~50.0 ng/m L质量浓度內呈现良好线性关系,R=0.999 9,方法的检出限为0.3μg/kg,回收率为89.9%~102.4%,相对标准偏差为1.8%~3.75%。该方法简单、快速、灵敏、净化效果好、回收率高,适合蔬菜中噻虫嗪农药残留的检测和安全监控。     

Selenium speciation analysis of Misgurnus anguillicaudatus selenoprotein by HPLC–ICP–MS and HPLC–ESI–MS/MS

Analytical methods for selenium (Se) speciation were developed using high-performance liquid chromatography (HPLC) coupled to either inductively coupled plasma mass spectrometry (ICP?CMS) or electrospray ionization tandem mass spectrometry (ESI?CMS/MS). Separations of selenomethionine (Se-Met) and selenocysteine (Se-(Cys)₂) with favorable peak shape and resolution were obtained by both HPLC-ICP-MS and HPLC?CESI?CMS/MS. Both methods achieved low limits of detection, high sensitivity and favorable stability. With HPLC?CESI?CMS/MS, signal suppression was observed when complex matrix was co-eluted, but excellent structural characterization was still achieved. Thus, HPLC-ICP-MS is better for the detection of Se species, and HPLC?CESI?CMS/MS is essential for molecular identification and confirmation. A water-soluble selenoprotein from purified M. anguillicaudatus muscle tissue was analyzed by the two complementary systems (HPLC-ICP-MS and HPLC?CESI?CMS/MS) with high sensitivity and accuracy. The results demonstrated that Se-Met was the predominant selenoamino acid in the purified selenoprotein from M. anguillicaudatus muscle tissue, and the concentration of Se-Met in the selenoprotein was 6.280?mg/kg (dry mass). In addition, in HPLC-ICP-MS, an unknown Se-containing compound with similar polarity to Se-(Cys)₂ was discovered. Using complementary data from HPLC?CESI?CMS/MS, it was determined that this unknown Se-containing compound was not Se(Cys)_2.     

Quantification of folpet and phthalimide in tea and herbal infusions by LC– high-resolution MS and GC–MS/MS

Two methods based on a modified QuEChERS sample preparation and either LC coupled to atmospheric pressure ionisation and high-resolution MS or GC coupled to electron ionisation and tripled quadrupole MS have been assessed for the quantification of folpet and phthalimide in tea and other dry herbal infusions. Both methods have been fully validated in green tea and further checked in black tea, verbena and rooibos, and they performed according to the SANTE/11813/2017 criteria at the target LOQ concentration level (50 µg/kg). These methods allow the accurate quantification of folpet in the selected matrices according to the new EU residue definition, which includes phthalimide. Phthalimide is the main metabolite and degradation product of folpet, although according to recent studies, it could be generated from different sources than folpet breakdown, such as food processing or analysis by GC.     

LC/MS/MS法测定白酒中氨基甲酸酯类农残研究

首次建立同时对蒸馏白酒中8种氨基甲酸酯类农药(抗蚜威、恶虫威、克百威、仲丁威、甲萘威、扑灭威、多菌灵、灭多威)残留的液相色谱串联质谱法(liquid chromatography-tandem mass spectrometry, LC/MS/MS)定性鉴别和定量测试方法,此8种农药残留的方法检出限为0.5 μg/kg^10 μg/kg。上述8种农药残留在蒸馏白酒中加标回收率为87.6 %~100.0 %,精密度为0.89 %~5.6 %,均能够满足测试要求。     

Rapid analysis of phenolic acids in beverages by UPLC–MS/MS

A rapid method for qualitative and quantitative analysis of 17 phenolic acids (gallic acid, 3,5-dihydroxybenzoic acid, protocatechuic acid, chlorogenic acid, gentisic acid, 4-hydroxybenzoic acid, caffeic acid, vanillic acid, syringic acid, 3-hydroxybenzoic acid, 4-coumaric acid, sinapic acid, ferulic acid, 3-coumaric acid, 2-coumaric acid, salicylic acid and trans-cinnamic acid) in different beverages was developed using ultra performance liquid chromatography (UPLC) coupled with tandem mass spectrometry (MS/MS). The analytes were detected in multiple reaction monitoring (MRM) mode and quantified using internal standards of deuterium-labelled 4-hydroxybenzoic (2,3,5,6-D4) and salicylic (3,4,5,6-D4) acids. Limits of detection (LODs) ranged from 0.15 to 15 pmol and the response was linear to 1000 pmol injected. Mean method precision of 4.4 RSD% (range, 2.0–9.1%) was obtained, and a mean accuracy (bias) of 1.1% (range, −14.5 to 17.5%). The applicability of this analytical approach was confirmed by the successful analysis of real samples of white wine, grapefruit juice and green tea infusion. Twelve phenolic acids were determined in the analysed beverages, in concentrations ranging from 40.8 to 9046 μg L⁻¹ and the results were compared to data from previous studies.     

MS La-Rio超高速数码印花机

介绍了数码印花的发展历史与现状、优势、发展瓶颈以及突破点。指出数码印花的发展经历了技术探索、打样定制、小批量生产和大批量生产4个阶段,其市场份额已经约占印花市场的4%;数码印花具有更短的生产周期,解决了传统印花高能耗、高排放的缺点,且在渐变色的表现上以及在丝绸、锦纶等弹性面料上,印花品质优势明显;伴随染料墨水的技术性突破,数码印花综合成本大大降低,成本瓶颈得到突破;另外由于打印喷头喷孔密度和喷头频率的改进,意大利MS公司MS La-Rio超高速数码印花机安装了220多颗京磁喷头,最快速度可约达75 m/min,每日极限产能达到10万m2以上,数码印花产能瓶颈也得到了突破。     

UPLC/MS/MS法测定饮料中甜蜜素、糖精钠和安赛蜜

建立了超高效液相色谱-串联质谱法(ultra high-performance liquid chromatography-tandem massspectrometry,UHPLC-MS/MS)测定饮料中甜蜜素、糖精钠和安赛蜜的检测方法。饮料加水稀释涡旋,用N-丙基乙二胺(PSA)净化样品,经0.22μm微孔滤膜过滤后测定甜蜜素;用乙酸锌-亚铁氰化钾净化样品,经0.22μm微孔滤膜过滤后测定糖精钠和安赛蜜。甜蜜素和安赛蜜在5～200μg/L、糖精在20～200μg/L范围内线性关系良好,方法检出限(S/N=3)为0.2～10μg/kg,方法定量限(S/N=10)为0.6～30μg/kg,3种化合物在奶茶中加标回收率为78.9%～95.7%,果茶中加标回收率为80%～102%。方法操作简单,检出限低,重现性好,回收率良好,干扰小。     

用HPLC/MS/MS仪定量分析烟丝和烟气中的TSNA

烟草特有亚硝胺 (TSNA)是所有烟草特有的成分。传统上采用带有热能分析器的气相色谱仪 (GC -TEA)测定烟丝和烟气中的TSNA ,该法的缺点是纯化步骤多 ,分析时间长。我们开发了一种替代传统GC -TEA的方法———HPLC/MS/MS法。本法仅涉及用含水溶剂对 2 5 0mg烟粉或收集主流烟气的剑桥滤片进行简单的萃取 ,勿需样品纯化步骤 ,且分析时间不到 10min。也即 ,在烟粉或收集烟气的剑桥滤片中加入氘化的内标物 ,振摇萃取 1h ,然后用带有正离子电子喷雾装置的HPLC/MS/MS仪进行分析。本法性能稳定 ,分析的样品数量大 ,数据可靠 (采用内标物 ) ,萃取效率高 ,加入烟样、滤片或烟气冷凝物中标样的相对回收率均为 95 %～ 10 5 %。检测限比传统分析方法低得多 ,每种TSNA的检测限均<0 .0 5ng/ml。此外 ,由于无样品纯化步骤且分析时间短 ,因此本法可在 2 4h内分析 10 0多个烟草或烟气样品     

水果中噻虫嗪农药残留LC/MS/MS测定

目的建立一种简单、快速、灵敏的水果中噻虫嗪农药残留的液相色谱-串联质谱(liquid chromatography-mass spectrometry/mass spectrometry,LC-MS/MS)分析方法。方法称取水果样品5 g,加入乙腈20 m L在超声波振荡条件下提取,提取液使用20 mg石墨化炭黑(Carb)和60 mg N-丙基乙二胺(PSA)粉末进行分散固相萃取净化,经液相色谱质谱联用仪检测,外标法定量。结果噻虫嗪农药残留的色谱图分离效果良好,方法的检出限为0.3μg/kg,线性相关系数为0.9999,噻虫嗪在苹果、梨、桃中的添加水平为0.01、0.05、0.10 mg/kg,回收试验表明该方法平均回收率为88.9%~100.3%(n=6),相对标准偏差为1.98%~4.53%。结论该方法简单、快速、灵敏、净化效果好、回收率高,适合水果中噻虫嗪农药残留的检测和安全监控。     

QuEChERS EMR-Lipid-LC/MS/MS测定8种β-受体激动剂

建立以QuEChERSEMR-Lipid为前处理测定动物源性食品中8种β-受体激动剂的LC-MS/MS方法。样品经粉碎混匀后加入pH为5.2乙酸-乙酸铵溶液,以β-盐酸葡萄糖醛酸苷酶/芳基硫酸酯酶酶解,酶解液经QuEChERSEMR-Lipid净化后,取乙腈层与0.1%的甲酸水溶液混合上LC-MS/MS进行分析。8种β-受体激动剂在测定浓度范围内线性关系良好,各组分相关系数R~20.998,加标回收率范围79.1%~94.8%,方法精密度范围5.4%~9.4%,测定各组分β-受体激动剂检出限范围0.2μg/kg~0.4μg/kg,定量限范围0.5μg/kg~1.0μg/kg。