生物组织中甲胺磷及其异构体的串联质谱法分析

目的建立可用于生物体内甲胺磷及其异构体O,O二甲基氨基硫代磷酸酯检验的高灵敏度方法。方法应用串联质谱法(GCMS/MS),对生物样品中的甲胺磷及其异构体进行检验研究。结果选择质荷比为141的离子为母离子,击发电压为0.8V时,甲胺磷及其异构体二次电离碎片适中,质谱谱图清晰。50%甲胺磷乳油进样量为0.1ng时,甲胺磷及O,O二甲基氨基硫代磷酸酯峰的信噪比分别为436、773。经实验,甲胺磷检测限为20pg。结论所拟方法能有效提高甲胺磷的检测灵敏度。     

肝中对硫磷的固相萃取—电子捕获检测气相色谱分析法

目的建立肝中对硫磷的快速、灵敏、可靠的GC／ECD分析方法。方法肝匀浆加内标甲基对硫磷,用乙腈浸提,浸提液加6％高氯酸稀释,稀释的上清液用GDX403树脂进行固相提取,提取物用HP-5色谱柱和电子捕获检测器进行气相色谱分析。结果提取率92.3％,检测限7.8ng／g,线性范围0.04～4.0μg／g,回收率99.6％±6.2％(Mean±CV,n=5)。结论方法简便、灵敏适合于实际案件检验。     

藏茴香中葛缕酮的含量测定

采用敢相色谱法藏茴香中葛楼酮含量，该法以联苯为内标物对葛缕酮进行定量测定，简单，快速，精确，。平均回收率为９９．６％，ＲＳＤ２．０％。     

超高效液相色谱-四级杆飞行时间串联质谱快速分析复方守宫散化学成分及血中移行成分

目的 采用超高效液相色谱-四级杆飞行时间质谱(ultra-performance liquid chromatogra-phy/quadrupole time-of-flight-tandem mass spectrometry,UPLC-Q-TOF/MS)对复方守宫散中化学成分及其血中移行成分进行定性分析,为该制剂的...     

气相色谱-质谱联用法分析 3种方法提取的三七挥发性成分

目的 运用气相色谱-质谱联用法对不同方法提取的三七挥发性成分进行比较分析。方法 分别采用回流提取法、超声提取法、静态顶空法提取三七挥发油,运用气相色谱-质谱联用技术,运用NIST11.0质谱数据库和峰面积归一化法对已分离的化合物进行鉴定并计算各成分的相对含量。结果 从回流提取、超声提取、静态顶空法提取的三七挥发油中分别鉴定出60、50、24个挥发性成分。在静态顶空法中相对质量分数最高的是香桧烯,占挥发性成分的24.97%;在回流提取法和超声提取法中相对质量分数最高的都是聚炔类物质环氧十三烷-4,11-二炔,分别占挥发性成分的9.97%和14.75%。首次从三七挥发性成分中鉴定出3个聚炔类化合物和2个甾体类化合物。结论 三七中挥发性成分主要为烷烃类、烯烃类、醛类、酸类、酯类、萜类、聚炔类、甾体类和杂环类物质。3种方法的补充利用可较全面地提取出三七中的挥发性物质。     

自制海洛因标准品在常用有机溶剂中稳定性研究

目的 研发海洛因标准品及优化分析方法,以对云南缴获海洛因样本提纯制备成的自制海洛因对照品在常用有机溶剂中的稳定性进一步研究.方法 采用内标及GC、GC/MS方法,通过对提纯制备的海洛因在5种有机溶剂中冷藏保存后含量的变化,观察海洛因在常用有机溶剂中的稳定性.结果 乙醇、三氯甲烷及乙腈为溶剂的自制海洛因对照品储备液,保存30天时间范围内海洛因含量未发生明显变化;以丙酮作为溶剂的自制海洛因对照品储备液,在7至30天时间范围内,海洛因含量明显升高;以甲醇作为溶剂的自制海洛因对照品储备液,在0小时至30天时间范围内,海洛因含量一直呈明显的下降趋势.结论 乙醇、三氯甲烷及乙腈可以作为海洛因样品储备液溶剂使用,丙酮、甲醇不适合作为海洛因样品储备液溶剂使用.     

3个道地产区黄芪中钙、镁、锌、铁、铜、锰含量测定

目的 测定3个道地产区黄芪中钙(Ca)、镁(Mg)、锌(Zn)、铁(Fe)、铜(Cu)、锰(Mn)的含量,以探讨道地药材与微量元素的相关性。方法 采用硝酸-过氧化氢（体积比5〖DK〗∶2）体系微波消解黄芪样品,火焰原子吸收光谱法测定黄芪中Ca、Mg、Zn、Fe、Cu、Mn的含量。结果 内蒙古黄芪除Cu元素含量稍低于山西黄芪之外,Ca、Mg、Zn、Fe、Mn元素含量都高于甘肃黄芪和山西黄芪;山西黄芪除Zn元素含量不低于甘肃黄芪之外,Ca、Mg、Fe、Cu、Mn元素含量都低于甘肃黄芪。结论 在内蒙古、甘肃、山西3个道地产区黄芪中,人体必需微量元素含量以内蒙古黄芪最优,甘肃黄芪次之,山西黄芪再次之。     

电感耦合等离子体质谱法测定金寨地区仿野生茯苓不同部位及其土壤中11种无机元素

目的 探究无机元素在金寨地区仿野生茯苓不同用药部位中的分布及在土壤中的富集特点。方法 采用微波消解法处理茯苓皮、白茯苓、赤茯苓及其菌核生长附近土壤,应用电感耦合等离子体质谱法测定茯苓不同部位及其土壤中K、Na、Mg、Fe、Mn、Zn、Cu、Se等11种无机元素含量。结果 金寨地区仿野生茯苓各部位元素分布有一定差异,大多数元素在茯苓皮中含量较高,茯苓不同部位总的无机元素含量从高至低顺序为茯苓皮、赤茯苓、白茯苓;茯苓不同部位对无机元素的吸收有选择性,但均以K、Fe、Mg、Na含量较高;茯苓不同部位对11种元素的富集系数存在差异,变化范围为0.005 2～0.782 3。结论 所建立的电感耦合等离子体质谱法简便、准确,适用于金寨地区仿野生茯苓不同部位及土壤中11种无机元素的含量测定。     

Potential for the Remediation of Methamphetamine Contamination Using Ozone,

The deposition of methamphetamine within indoor environments due to illegal activities can pose a health risk for occupants. Current cleaning techniques are costly and inefficient, calling for the development of alternative remediation methods. In addition, the fate of methamphetamine in indoor environments is largely unknown, negatively impacting our knowledge on the health risks associated with contaminated dwellings. Under the conditions of this study, 97% of surface deposited methamphetamine on a paper substrate was consumed after 12 min of exposure to ozone, thus demonstrating potential for its use as a remediation agent. The reaction had an effective second‐order rate constant with an upper limit of 2.15 ± 1 × 10^?18 cm³/molecule/s, and the main product observed was phenyl‐2‐propanone (P2P) at 8.3% yield, as determined using GC/MS. Several products observed in this study have also been reported as by‐products of methamphetamine synthesis, including P2P—a known methamphetamine precursor, which indicates that their detection at a potential clandestine site is not necessarily evidence of manufacture.     

Carbon‐Based Fingerprint Powder as a One‐Step Development and Matrix Application for High‐Resolution Mass Spectrometry Imaging of Latent Fingerprints

Carbon‐based materials are often used as matrices for matrix‐assisted laser desorption/ionization mass spectrometry (MALDI‐MS) and its imaging (MALDI‐MSI). However, researchers have refrained from using carbon‐based fingerprint powder (CFP) as a matrix due to high background and contamination. In this work, the compatibility of CFP is reevaluated with MALDI‐MSI using a high‐resolution mass spectrometer (HRMS) and compared to traditional organic matrices. Relevant fingerprint compounds were easily distinguished from carbon cluster peaks when using HRMS. For fair comparison, half of a fingerprint was dusted with CFP while the other half was dusted with traditional organic matrices. All compounds studied had comparable, or higher, signal‐to‐noise (S/N) ratios when CFP was used as the matrix. Additionally, chemical image qualities closely followed the trend of S/N ratios. CFP proved to be an effective one‐step development and matrix application technique for MALDI‐MSI of latent fingerprints, when carbon cluster peaks are well separated by a HRMS.