N-亚硝基芬氟拉明的液相色谱-质谱/质谱联用检测及化学合成

建立了芬氟拉明衍生物的液相色谱-质谱/质谱联用(LC-MS/MS)检测方法,对其中一个衍生物进行化学合成,并经过LC-MS/MS和~1H NMR表征。     

高效液相色谱-质谱联用技术在药物分析中的应用

介绍了近年来高效液相色谱-质谱接口技术的研究进展,综述了该技术在中药指纹图谱研究、药物代谢分析、药物中非法添加化学药物成分的鉴定分析、以及残留药物成分的鉴定分析方面的应用。随着液质联用技术的不断完善、发展,其必将在药物分析中发挥越来越重要的作用。     

高效液相色谱-质谱串联法测定化妆品中的邻苯二甲酸酯

应用高效液相色谱-质谱串联法检测化妆品中的邻苯二甲酸酯,检测出化妆品中11种邻苯二甲酸酯类化合物,对化妆品中的检测物质进行甲醇超声震荡提取,采用Endeavorsil C18液相色柱进行分离,并进行串联质谱检测。该方法具有高效的灵敏度和精密度,在化妆品中的邻苯二甲酸酯检测工作中具有一定应用价值。     

甲霜灵试纸实地检测与液相色谱-质谱联用比对结果分析

报道了甲霜灵胶体检测试纸实地应用的验证研究成果. 甲霜灵胶体金检测试纸的实地检测与液相色谱-质谱联用法(LC/MS -MS)比对试验结果显示两种方法得出的检测结果相一致. 检测试纸可作为蔬菜采摘前农药甲霜灵残留自我检测手段的应用,从而实现对甲霜灵农药残留的源头把关.     

0.006%冠菌素SL高效液相色谱-质谱的分析方法

[目的]建立一种适用于低浓度的植物生长调节剂0.006%冠菌素SL中有效成分HPLC-MS的分析方法。[方法]以乙腈和0.1%甲酸水作为流动相(体积比50∶50),0.5 mL/min流速,通过ESI离子源正离子的扫描模式,定量分析0.006%冠菌素SL有效成分含量。[结果]该定量分析方法的决定系数R²为0.9964,标准偏差为0.004,变异系数0.4%,回收率在99.10%～100.60%之间,平均回收率为99.72%。[结论]该分析方法操作简单,并且精密度较好、准确度较高,且具有良好的线性相关性,可准确分析0.006%冠菌素SL有效成分含量。     

10%噁嗪草酮悬浮剂高效液相色谱串联质谱分析

为建立一种利用高效液相色谱-质谱测定10%噁嗪草酮悬浮剂含量的方法。利用ESI离子源在正离子模式下扫描。结果表明,当乙腈与0.1%甲酸体积比80∶20、柱温35℃、流速1 mL/min时噁嗪草酮峰型及峰面积及保留时间最优。在该方法下线性关系R²系数为0.999 9,标准偏差为0.087,加标回收率为98.235%～100.57%。采用该种液质联用方法更加便捷、准确、可靠,可以快速检测分析10%噁嗪草酮悬浮剂含量。     

超高效液相色谱-串联质谱技术同时分析食品中多种植物激素残留

[目的]建立食品中多种植物激素残留量检测的超高效液相色谱-串联质谱的分析方法。[方法]样品经甲醇-水(体积比90∶10)提取,浓缩后经WCX小柱净化,采用Waters C18色谱柱分离,以乙腈和0.1%甲酸水溶液为流动相进行梯度洗脱,采用电喷雾-正离子多反应监测模式,外标法定量。[结果]在1～100μg/L的质量浓度范围内,各种植物激素相关系数均大于0.997,该方法的检出限在0.3～0.5μg/kg之间,定量限在1.0～1.5μg/kg之间。添加水平5～20μg/kg范围内,7种植物激素的回收率在80.2%～119.3%之间,日内和日间相对标准偏差在0.65%～7.28%之间。[结论]该方法简单、灵敏度高、分析时间短,适用于多种植物激素的测定。     

高效液相色谱-电喷雾质谱联用研究三氯生的光聚合产物

三氯生在光解时可能会产生二(噁)英类物质,因而它在日用化学品中的安全性受到学术界的广泛关注.本文采用高效液相色谱-电喷雾质谱研究了三氯生在紫外光照射下的光聚合反应,通过对产物的准分子离子分析,初步确定了7种光聚合产物.聚合物的分子离子分别为505、540、792,且有同分异构体存在,其异构体个数分别为2个、3个和2个.这些物质的产生主要由三氯生分子间脱除氯化氢、分子上脱除氯离子等过程来聚合完成.在光解溶液中也测到2,8-二氯代二苯并-对-二(噁)英,该物质则是通过分子自身脱除氯化氢而环化产生.同时应用液相色谱定性分析了不同光源对光聚物产生及含量变化的影响.结果表明,三氯生的光聚合反应受光源的影响显著,UVB比UVA更易产生聚合反应.     

Determination of Oxidized Phosphatidylcholines by Hydrophilic Interaction Liquid Chromatography Coupled to Fourier Transform Mass Spectrometry

A novel liquid chromatography-mass spectrometry (LC-MS) approach for analysis of oxidized phosphatidylcholines by an Orbitrap Fourier Transform mass spectrometer in positive electrospray ionization (ESI) coupled to hydrophilic interaction liquid chromatography (HILIC) was developed. This method depends on three selectivity criteria for separation and identification: retention time, exact mass at a resolution of 100,000 and collision induced dissociation (CID) fragment spectra in a linear ion trap. The process of chromatography development showed the best separation properties with a silica-based Kinetex column. This type of chromatography was able to separate all major lipid classes expected in mammalian samples, yielding increased sensitivity of oxidized phosphatidylcholines over reversed phase chromatography. Identification of molecular species was achieved by exact mass on intact molecular ions and CID tandem mass spectra containing characteristic fragments. Due to a lack of commercially available standards, method development was performed with copper induced oxidation products of palmitoyl-arachidonoyl-phosphatidylcholine, which resulted in a plethora of lipid species oxidized at the arachidonoyl moiety. Validation of the method was done with copper oxidized human low-density lipoprotein (LDL) prepared by ultracentrifugation. In these LDL samples we could identify 46 oxidized molecular phosphatidylcholine species out of 99 possible candidates.     

液相色谱-电喷雾串联四极杆质谱测定水果中的丁酰肼

建立了4种水果中丁酰肼残留量的液相色谱-电喷雾串联四极杆质谱检测方法.样品经匀浆提取净化后.采用LC-MS/MS法,ESI(+)电离方式,多反应监测(MRM)定量,用Vensil HILIC色谱柱,以含0.1%甲酸的水和乙腈为流动相进行洗脱.结果表明:丁酰肼在0.01～1.0 mg/L质量浓度范围内呈现良好的线性,相关系数为0.999 1,方法的检出限为2.5 μg/kg,当添加质量分数为0.01、0.1、0.5 mg/kg时,4种水果中丁酰肼的平均回收率为77.7%～103.7%,相对标准偏差为2.0%～9.3%.     

Liquid Chromatography–High-Resolution Mass Spectrometry for Quantitative Analysis of Gangliosides

Gangliosides are a large family of glycosphingolipids that are abundant in the brain, and have been shown to affect neuronal plasticity during development, adulthood, and aging. We developed a fast, efficient, and sensitive liquid chromatography–mass spectrometry method to quantify eight different classes of gangliosides (GM₁, GM₂, GM₃, GD₃, GD_1a, GD_1b, GT_1b, GQ_1b) in the brains of 2-day-old and 80-day-old Wistar rats. The gangliosides were extracted from rat brain using a modified Svennerholm and Fredman method. After ganglioside class separation using a hydrophilic high performance liquid chromatography (HPLC) column, the resolving power of the LTQ-Orbitrap™ mass spectrometer was used to extract and sum the major species of each ganglioside class, generating fully resolved extracted ion current peaks for both standards and samples. The flexibility and the specificity of this method are such that it can be applied to the analysis of other ganglioside species/classes not discussed in this paper, provided appropriate standards are available. The method had good repeatability (coefficient of variation 4.8–12.3%) and mean recoveries in the range 92–107%.     

HPLC-MS/MS测定化妆品中的NDELA

化妆品以d8-NDELA为内标,经提取净化后,采用HPLC-MS/MS测定NDELA(N-亚硝基二乙醇胺)。提取净化时水溶性样品以水作溶剂,用C18柱固相萃取,水不溶性样品用二氯甲烷进行液液萃取。该方法线性范围为5.0 ng/mL～80 ng/mL,NDELA定量限为50μg/kg,回收率85%～104%。实验结果表明,该方法灵敏、准确、重复性好。     

液相色谱及液质联用技术在环境分析中的应用

高效液相色谱（HPLC）是在经典液相色谱法和气相色谱法的基础上发展起来的新型分离分析技术。20世纪80、90年代后,HPLC技术发展迅速,特别是21世纪初,液相色谱与现代质谱的联机技术有了很大的发展,使HPLC的应用前景更为广阔。在全部已知的有机化合物中近80％的有机化合物属于挥发性低,易受热分解或者大分子化合物,适合于高效液相色谱进行分析。本文主要从HPLC分析方法的特点为切入点,介绍液相色谱及液质联用技术在环境分析中的应用。     

液相色谱-串联质谱法测定化妆品中米诺地尔的含量

提出了液相色谱-串联质谱联用法测定化妆品中米诺地尔含量的方法。样品经甲醇超声提取,用高效液相色谱分离后,采用电喷雾串联质谱进行定性和定量检测。线性范围为2～100ng·mL-1,线性相关系数r大于0．99,方法的检出限为2g·kg-1（S／N=10）,高、中、低3个浓度水平的加标回收率在90％～110％o之间,测定值的相对标准偏差（n=6）小于10％。     

液相色谱-串联质谱法测定化妆品中地索奈德-21-醋酸酯

建立了液相色谱-串联质谱法测定化妆品中糖皮质激素地索奈德-21-醋酸酯的方法。样品经甲醇超声提取,通过SPE小柱净化,利用Poroshell 120 SB C18(1.8μm,2.1×75 mm)色谱柱分离,以0.1%甲酸水溶液和0.1%甲酸乙腈溶液为流动相,梯度洗脱。在电喷雾离子源的正离子模式下采用多反应监测(MRM)模式采集数据并进行测定。在优化的条件下,地索奈德-21-醋酸酯在10~200μg/mL范围内线性关系良好,相关系数大于0.999。在0.1、0.5、2.0μg/g 3个浓度加标水平下,平均回收率为90.1%~94.9%,相对标准偏差为1.4%~2.8%,检出限(S/N=3)为0.03μg/g,定量限(S/N=10)为0.10μg/g。该方法准确可靠、快速灵敏,可用于化妆品中地索奈德-21-醋酸酯的测定。     

氯霉素残留的液相色谱质谱检测方法的样品前处理研究进展

氯霉素能抑制骨髓造血功能和引起再生障碍性贫血等毒副作用,包括中国在内的多个国家把它列为违禁药物,禁止在动物食品中检出,本文综述了氯霉素残留的液相色谱质谱检测方法的样品前处理方法,包括直接提取法,固相萃取法,Qu ECh ERS方法。     

Comprehensive Steroid Assay with Non-Targeted Analysis Using Liquid Chromatography Ion Mobility Mass Spectrometry

Aldosterone-producing adenomas (APAs) have different steroid profiles in serum, depending on the causative genetic mutation. Ion mobility is a separation technique for gas-phase ions based on their m/z values, shapes, and sizes. Human serum (100 µL) was purified by liquid–liquid extraction using tert-butyl methyl ether/ethyl acetate at 1/1 (v/v) and mixed with deuterium-labeled steroids as the internal standard. The separated supernatant was dried, re-dissolved in water containing 20% methanol, and injected into a liquid chromatography–ion mobility–mass spectrometer (LC/IM/MS). We established a highly sensitive assay system by separating 20 steroids based on their retention time, m/z value, and drift time. Twenty steroids were measured in the serum of patients with primary aldosteronism, essential hypertension, and healthy subjects and were clearly classified using principal component analysis. This method was also able to detect phosphatidylcholine and phosphatidylethanolamine, which were not targeted. LC/IM/MS has a high selectivity for known compounds and has the potential to provide information on unknown compounds. This analytical method has the potential to elucidate the pathogenesis of APA and identify unknown steroids that could serve as biomarkers for APA with different genetic mutations.     

液相色谱—质谱联用技术在中药刺五加分析中的应用

液相色谱-质谱联用技术(HPLC-MS)是利用液相色谱高效分离和质谱强大的结构检测结合的联用技术,该技术检测灵敏度高、选择性强,在各个领域应用范围广泛,尤其在中药产物结构鉴定中发挥重要作用,可以实现中药成分分析、结构分析、含量分析等过程。刺五加中具有较高的药用价值,可以调节人体免疫、抗辐射、抗癌等作用,文章采用液相色谱-质谱联用技术分析刺五加中活性成分及结构,结果表明刺五加中主要包括黄酮类的槲皮素、槲皮苷、芦丁以及皂苷类的刺五加苷D及刺五加苷异构体E,刺五加苷A,刺五加苷B等,以其对中药刺五加的现代化分析提供一定的技术支持。