解吸电喷雾质谱法协同主成分分析快速鉴定红茶茶水

茶叶的快速鉴定对于茶叶的高效生产和品质控制十分重要.目前茶叶品质主要依赖于专业评茶师主观鉴定,亟待建立快速、准确的仪器方法进行客观评价.解吸电喷雾(DESI)质谱法是一种新型快速的质谱分析方法,在农产品和日用品的快速检测上有着很强的应用优势.本文采用解吸电喷雾质谱法和主成分分析方法对外观相近的三个品牌红茶产品进行了分析.结果表明,该方法能够快速清晰地分辨不同品牌的红茶产品,有着良好的应用前景.     

DART-MS快速检测中药材中非法染色物质金胺0

采用实时直接分析质谱法(DART-MS),建立了能直接对中药材及其饮片中非法添加金胺0快速进行定性的检测方法。在简单的样品预处理的情况下,方法检出限为50 ng,单个样品的检测时间不超过30 s。方法可用于中药材中金胺0的非法添加定性分析。     

毛细管区带电泳法分离测定磺胺药物残留综合实验设计与实践*

结合科研项目,选取学生熟悉的实际样品设计了一个适用于本科教学的仪器分析综合实验——毛细管区带电泳法分离测定磺胺药物残留综合实验设计与实践。详细展示了土壤样品、茶叶样品中磺胺类药物残留完整的分离分析的实验教学过程:首先学生利用有机化学知识对磺胺标准品衍生化,对实际样品进行预处理,然后借助仪器分析化学知识展开分组讨论,从缓冲液浓度、pH、温度等方面探究毛细管电泳分离分析磺胺类药物残留的最优条件,自主设计迁移时间、峰面积重现性实验和加标回收率实验考察实验重现性、精密度,并根据实验实时融入食品、药品安全课程思政。据此培养学生运用综合知识分析和解决实际问题能力、团队分工协助意识和严谨的实验态度,打破科研与教学的壁垒,实现科研对实验教学的带动作用。     

实时直接分析质谱法快速鉴别天然驱蚊产品中的人工添加剂

采用DART-MS(实时直接分析质谱法)建立了一种简单快速测定人工合成驱蚊化合物如DEET(避蚊胺)、BAAPE(驱蚊酯)等的方法.在常温常压下,无需对天然驱蚊产品进行任何预处理,通过比对标准品的质谱信号离子,即可快速鉴别出天然驱蚊产品中的人工添加剂.该方法大大缩短了分析时间,并且具有原位、准确且高通量的优点.     

赛默飞推出高效液相色谱法快速测定茶叶中嘧霉胺的解决方案

<正>赛默飞世尔科技近日推出高效液相色谱法快速测定茶叶中嘧霉胺的解决方案。嘧霉胺是近年来开发的一种结构新颖、作用机制独特的嘧啶胺类内吸性杀菌剂,主要用于灰霉病的防治。嘧霉胺的常见测定方法有气相色谱法、气相质谱法、高效液相色谱法和高效液相质谱法。样品的前处理是茶叶中嘧霉胺测定的关键步骤之一。Qu ECh ERS是"快速、简易、廉价、有效、稳定、安全"的萃取方法。该方法利用乙腈萃取     

合成卡西酮类新精神活性物质检测方法的应用进展

鉴于2010年以来有关合成卡西酮类新精神活性物质检测方法的综述较少，简要介绍了合成卡西酮类新精神活性物质的分类和药理作用，并综述了化学分析法、免疫学检测法、光谱分析法、核磁共振波谱法、毛细管电泳法、液相色谱法、气相色谱-质谱法、液相色谱-质谱法和实时直接分析质谱法等在该类毒品检测中的应用，并对相关检测方法的发展进行了展望(引用文献57篇)。     

环境样品中铀的HR-ICP-MS测定

高分辨电感耦合等离子体质谱法(HR-ICP-MS)是痕量元素分析的有效手段。本文采用HR-ICP-MS对环境样品(土壤、底泥、茶叶、地表水)中铀浓度和同位素比值进行了测定。土壤、底泥、茶叶样品采用微波消解法进行溶解;水样采用45μm滤膜过滤后直接测定。实验对样品制备、仪器参数设定、记忆效应消除、质量歧视效应修正等进行了探索,建立了环境样品中痕量铀浓度和同位素比值测定方法。土壤制样过程中铀的加标回收率为97.7%,铀检出限0.51ng·L~(-1)。     

单光子电离质谱法在线分析牙膏中的香精物质

在无需样品前处理的条件下,建立了直接进样单光子电离飞行时间质谱在线分析牙膏样品中香精物质的方法。本方法采用石英毛细管直接将样品导入质谱仪电离区,优化了电离区气压条件,并利用香精标准品的特征质谱信号对牙膏样品中香精成分进行了快速、准确鉴定,单个样品分析仅需0.5 min。将本方法应用于模拟刷牙过程中挥发性香精的在线、原位监测,考察了水含量对牙膏香精挥发过程的影响。结果表明,直接进样单光子电离飞行时间质谱法能够实时监控刷牙过程中挥发香精的成分与浓度,可以应用于其他样品如食品、化妆品中香精成分的分析。     

茶叶中高氯酸盐检测方法研究进展

茶叶中新型污染物高氯酸盐在近年来受到越来越多的关注,相应的检测技术也在不断加强.参考国内外文献,综述了茶叶中高氯酸盐的检测方法.目前,茶叶中高氯酸盐的检测方法主要有离子色谱法（IC）、离子色谱-质谱法（IC-MS）和高效液相色谱-串联质谱法（LC-MS-MS）.比较了不同检测方法的局限性和优越性,重点比较了高效液相色谱-串联质谱法不同前处理方法、净化小柱和检测条件的优劣,对茶叶高氯酸盐检测技术的发展和研究进行了展望,为检测茶叶中高氯酸盐的新材料研发和检测新标准的建立提供理论依据.     

分光光度法测定桂西茶叶中铁的含量

茶叶既是食品,又是一味传统医药用的中药,药食同源.用分光光度法直接测定了茶叶中铁的含量,方法简便、快速、准确,对指导人们合理饮用茶叶进行补铁及进一步开发茶叶提供了可靠的理论依据.     

Rapid detection of bacterial endotoxins in ophthalmic viscosurgical device materials by direct analysis in real time mass spectrometry

Bacterial endotoxins are lipopolysaccharides bound to the bacterial cell wall and released when bacteria rupture or disintegrate. Possible contamination of endotoxin in ophthalmic devices can cause a painful eye inflammation or result in toxic anterior segment syndrome after cataract surgery. Measurement of bacterial endotoxin in medical device materials is difficult since endotoxin binds with polymer matrix and some of the materials are very viscous and non-water soluble, where traditional enzyme-based Limulus amebocyte lysate (LAL) assay cannot be applied. Here we propose a rapid and high throughput ambient ionization mass spectrometric (MS) method using direct analysis in real time (DART) for the evaluation of endotoxin contamination in medical device materials. Large and structurally complex endotoxin instantaneously breaks down into low-mass characteristic fragment ions using DART and is detected by MS in both positive and negative ion modes. This method enables the identification and separation of endotoxin from medical materials with a detection limit of 0.03 ng mL⁻¹ endotoxins in aqueous solution. Ophthalmic viscosurgical device materials including sodium hyaluronate (NaHA), non-water soluble perfluoro-n-octane (PFO) and silicone oil (SO) were spiked with different known concentrations of endotoxin and analyzed by DART MS, where the presence of endotoxin was successfully detected and featured small mass fragment ions were generated for NaHA, PFO and SO as well. Current findings showed the feasibility of measuring endotoxin contamination in medical device materials using DART-MS, which can lead to a one-step analysis of endotoxins in different matrices, avoiding any potential contamination during sample pre-treatment steps.     

分散固相萃取-分散液液微萃取结合气相色谱-三重四极杆质谱法测定茶叶中7种拟除虫菊酯类农药残留

将分散固相萃取和分散液液微萃取(d-SPE-DLLME)相结合,并与气相色谱-三重四极杆质谱(GC-MS/MS)联用,建立了快速测定茶叶中7种拟除虫菊酯类农药残留的方法。样品经乙腈提取,N-丙基乙二胺(PSA)和多壁碳纳米管(MWCNTs)净化,四氯化碳(CCl_4)浓缩萃取后,采用GC-MS/MS进行分析。以全发酵红茶为基质,考察了提取剂种类、萃取剂的种类和体积、分散剂体积以及萃取时间对萃取效率的影响。以乙腈为提取剂进行分散固相萃取,在进行分散液液微萃取时,以200μL CCl4为萃取剂,1 m L乙腈为分散剂,萃取时间为1 min。结果表明,7种拟除虫菊酯类农药在10~500μg/kg浓度范围内线性关系良好,定量下限为1.0~10.0μg/kg。7种农药在4种茶叶(红茶、绿茶、乌龙茶和黑茶)中4个添加水平下的平均回收率为75.4%~113.6%,相对标准偏差(RSD,n=5)不大于8.8%。该方法具有简单、快速、成本低、检出限低的特点。应用所建立的方法对12种市售茶叶样品进行检测,结果满意。     

Rapid qualitative analysis of 2 flavonoids,rutin and silybin,in medical pills by direct analysis in real‐time mass spectrometry (DART‐MS) combined with in situ derivatization

Direct analysis in real‐time mass spectrometry (DART‐MS) with in situ silylation was used for the rapid analysis of the flavonoids silybin ((2R,3R)‐3,5,7‐trihydroxy‐2‐[3‐(4‐hydroxy‐3‐methoxyphenyl)‐2‐hydroxymethyl‐2,3‐dihydrobenzo[1,4]dioxin‐6‐yl]chroman‐4‐one) and rutin (quercetin‐3‐O‐rutinoside). Three different derivatization reagents, hexamethyldisilazane/trimethylchlorosilane/pyridine (HMDS/TMCS/pyridine), N,O‐bis(trimethylsilyl)acetamide/trimethylchlorosilane/N‐trimethylsilyimidazole (BSA/TMCS/TMSI), and N,O‐bis(trimethylsilyl)trifluoroacetamide/trimethylchlorosilane (BSTFA/TMCS), were applied. Silybin and rutin were detected with various degrees of silylation, and the formation of dimers with pyridine and imidazole was also observed. HMDS/TMCS/pyridine was the best choice for the DART‐MS analysis of silybin, and BSA/TMCS/TMSI was the most effective for the detection of rutin. The effects of the DART source temperature on desorption, ionization, in‐source fragmentation, dimer formation, and hydrolysis of the trimethylsilyl groups were also studied. In addition, the collision‐induced dissociation properties of the derivatized silybin and rutin were explored. With our in situ silylation method, the derivatized bioactive compounds in intact medical pills could also be detected by DART‐MS.     

实时直接分析高分辨质谱技术研究碳硼烷类化合物

该文运用高分辨质谱技术对实时直接分析(Direct analysis in real time,DART)离子化条件下碳硼烷化合物的质谱行为进行了研究,对碳硼烷化合物DART高分辨质谱中所得到的同位素峰簇进行了表征与归属。研究结果表明,选取的碳硼烷化合物在DART负离子条件下均能得到较好的质谱信号,这可能与硼笼结构的“缺电性”有关。含10个B原子的碳硼烷化合物形成的离子同位素峰簇信号中,通常情况下相对丰度最高的同位素峰中含2个10B以及8个11B。将碳硼烷化合物高分辨质谱分析的精确m/z数据信息与图谱中同位素峰轮廓分析相结合,是碳硼烷化合物有效的质谱定性分析与表征策略。     

The coupling of direct analysis in real time ionization to Fourier transform ion cyclotron resonance mass spectrometry for ultrahigh‐resolution mass analysis

Direct Analysis in Real Time (DART) is an ambient ionization technique for mass spectrometry that provides rapid and sensitive analyses with little or no sample preparation. DART has been reported primarily for mass analyzers of low to moderate resolving power such as quadrupole ion traps and time‐of‐flight (TOF) mass spectrometers. In the current work, a custom‐built DART source has been successfully coupled to two different Fourier transform ion cyclotron resonance (FT‐ICR) mass spectrometers for the first time. Comparison of spectra of the isobaric compounds, diisopropyl methylphosphonate and theophylline, acquired by 4.7 T FT‐ICR MS and TOF MS, demonstrates that the TOF resolving power can be insufficient for compositionally complex samples. 9.4 T FT‐ICR MS yielded the highest mass resolving power yet reported with DART ionization for 1,2‐benzanthracene and 9,10‐diphenylanthracene. Polycyclic aromatic hydrocarbons exhibit a spatial dependence in ionization mechanisms between the DART source and the mass spectrometer. The feasibility of analyzing a variety of samples was established with the introduction and analysis of food products and crude oil samples. DART FT‐ICR MS provides complex sample analysis that is rapid, highly selective and information‐rich, but limited to relatively low‐mass analytes. Copyright © 2010 John Wiley & Sons, Ltd.     

Combination of Solid‐Phase Micro‐Extraction and Direct Analysis in Real Time‐Fourier Transform Ion Cyclotron Resonance Mass Spectrometry for Sensitive and Rapid Analysis of 15 Phthalate Plasticizers in Beverages

A method for rapid identification and quantification of phthalate plasticizers in beverages was developed. A number of 15 phthalate plasticizers which covered all the phthalates concerned in the US Consumer Product Safety Improvement Act (CPSIA), European Union legislations and Chinese national standards (GB) were analyzed. By a combined solid‐phase micro‐extraction (SPME) and direct analysis in real time mass spectrometry (DART‐MS) approach, phthalates at sub‐ng·mL^?1 levels can be qualitatively and quantitatively analyzed in a short time. The use of ultrahigh‐resolving power and the accurate mass measurement capacity naturally provided by Fourier transform ion cyclotron resonance mass spectrometry (FT‐ICR‐MS) minimizes the matrix interferences and thus enables the evaluation of phthalates in a complex matrix without extensive sample handlings or preparations. The limits of quantification (LOQs) were estimated to be at 0.3–5.0 ng·mL^?1, lower than the Maximum Residue Limit (MRL) regulated by the European Union legislations (2007/19/EC) in foods, beverages, food packaging and toys (0.3–30 ng·mL^?1). This rapid and easy‐to‐use SPME‐DART‐FT‐ICR‐MS method provided a relatively high‐throughput and powerful analytical approach for quick testing and screening phthalates in beverages and water samples to ensure food safety.     

Rapid direct analysis in real time (DART) mass spectrometric detection of juvenile hormone III and its terpene precursors

Direct analysis in real time (DART) is a plasma-based ambient ionization technique that enables rapid ionization of small molecules with high sample throughput. In this work, DART was coupled to an orthogonal (oa) time-of-flight (TOF) mass spectrometer and the system was optimized for analyzing a vital hormonal regulator in insects, juvenile hormone (JH) III and its terpene precursors, namely, farnesol, farnesoic acid, and methyl farnesoate. Optimization experiments were planned using design of experiments (DOE) full factorial models to identify the most significant DART variables contributing to JH III analysis sensitivity by DART-TOF mass spectrometry (MS). The optimized DART-TOF MS method had femtomole to sub-picomole detection limits for terpene standards, along with mass accuracies below 5 ppm. Finally, the possibility of distinguishing between two farnesol isomers by in-source-collision-induced dissociation (CID) in the first differentially pumped region of the oaTOF mass spectrometer was investigated. DART-MS enabled high-throughput, sensitive analysis with acquisition times ranging from 30 s to a minute. To the best of our knowledge, this is the first report on the application of DART-MS to the detection and identification of volatile or semi-volatile insect terpenoids, and on the use of DOE approaches to optimize DART-MS analytical procedures.     

实时直接分析-串联质谱法快速筛查火锅底料、牛肉面汤及调味料中罂粟壳生物碱

建立了采用实时直接分析-串联质谱(DART-MS/MS)对火锅底料、牛肉面汤及调味料中5种非法添加的罂粟壳生物碱进行快速筛查的方法。样品经乙腈提取净化后,在离子化温度为300℃、栅极电压为150 V、进样速率为0.8 m m/s的DART离子源正离子模式条件下进样,以电喷雾离子源正离子多反应监测(MRM)模式进行检测,实现了样品经简单预处理后使用DART-MS/MS进行检测的新方法。该方法简便、快速,能满足大批量非法添加样品的快速筛查分析要求。     

实时直接分析电离质谱法快速检测化妆品中的3种成分

建立用于化妆品中违禁成分尿刊酸(URA)、准用防晒剂甲氧基肉桂酸乙基己酯(EHMC)、丁基甲氧基二苯甲酰基甲烷(B-MDM)快速检测的快速检测方法。 采用实时直接分析(DART)离子源结合四极杆飞行时间质谱(Q-TOF MS),在正离子模式下,采用Full scan扫描方式,将化妆品样品直接置于离子化区域内进行快速定性分析。 在定量分析时,采用筛网模块进样,对实验参数进行系统优化,测得3种成分的定量范围在25～1000 mg/L之间,线性关系良好(r＞0.99),该方法的最低检出限(S/N=3)为7.5 mg/L,最小定量限(S/N=10)为25 mg/L,方法回收率在96.7%～109.2%之间,精密度RSD(n=6)为3.59%～11.23%。 该方法操作简单、快捷高效、环保绿色,可广泛应用于化妆品中化妆品中违禁防晒剂及添加剂的快速筛查与定量检测。     

Optimization of a direct analysis in real time/time-of-flight mass spectrometry method for rapid serum metabolomic fingerprinting

Metabolomic fingerprinting of bodily fluids can reveal the underlying causes of metabolic disorders associated with many diseases, and has thus been recognized as a potential tool for disease diagnosis and prognosis following therapy. Here we report a rapid approach in which direct analysis in real time (DART) coupled with time-of-flight (TOF) mass spectrometry (MS) and hybrid quadrupole TOF (Q-TOF) MS is used as a means for metabolomic fingerprinting of human serum. In this approach, serum samples are first treated to precipitate proteins, and the volatility of the remaining metabolites increased by derivatization, followed by DART MS analysis. Maximum DART MS performance was obtained by optimizing instrumental parameters such as ionizing gas temperature and flow rate for the analysis of identical aliquots of a healthy human serum samples. These variables were observed to have a significant effect on the overall mass range of the metabolites detected as well as the signal-to-noise ratios in DART mass spectra. Each DART run requires only 1.2 min, during which more than 1500 different spectral features are observed in a time-dependent fashion. A repeatability of 4.1% to 4.5% was obtained for the total ion signal using a manual sampling arm. With the appealing features of high-throughput, lack of memory effects, and simplicity, DART MS has shown potential to become an invaluable tool for metabolomic fingerprinting.