建立了非那西丁的气相色谱/质谱/质谱(GC/MS/MS)联用检测血中去痛片的主要代谢物非那西丁的新方法。采用液液提取法,用乙醚提取血中非那西丁,提取物水浴浓缩后进行GC/MS和GC/MS/MS分析,检测总离子流色谱(TIC)和一级质谱,并以非那西丁一级质谱基峰为母离子的测定其二级质谱,体内药物用GC/MS全扫描定性分析即用二级质谱结合其总离子流色谱峰的保留时间定性;选择离子扫描定量分析,采用内标曲线法,根据非那西丁和内标SKF525A二级质谱的TIC峰面积比进行定量分析。

A new method was developed for the analysis of 2,6-diethylaniline(2,6-DEA), the major metabolite of alachor, in urine by heptafluorobutyryl (HFB) derivatization-gas chromatography/tandem mass spectrometry(GC/MS/MS). After urine samples were extracted with cyclohexane, the extracts were derivatized with heptafluorobutyrylchloride ( HFBC) , and then the total ion chromagrams( TIC) , mass spectra and tandem mass spectra of derivatives were acquired. 2 ,6-DEA was identified by the tandem mass spectra and the retention time of its TIC chromatograms. Using 2 , 5-dichloroaniline as the internal standard, quantification was performed according to the peak area ratio of the TIC peak from tandem mass spectrometry of the derivatives of 2 ,6-DEA and internal standard. The internal standard calibration curve of 2 ,6 DEA derivative was used in quantification. The method was sensitivity and accurate for the qualitative and quantitative analysis of 2 ,6-DEA in urine samples. The extraction e

建立了气相色谱串联质谱法鉴别多氯联苯二代污染物羟基多氯联苯的方法,并用于水产品中羟基多氯联苯的分析。在60℃下,羟基多氯联苯经硅烷化衍生40min,在气相色谱三重四级杆串联质谱仪全扫描模式（Fullscanmode）下进行扫描,得到一级质谱全扫描图谱,确定3-羟基-多氯联苯101（3-OH-PCB101）、4-羟基-多氯联苯106（4-OH-PCB106）、4-羟基-多氯联苯112（4-OH-PCB112）等7种衍生化合物丰度最高的碎片离子,以此碎片离子为母离子,在二级质谱多反应监测模式（MRM）下进行扫描,得到二级质谱全扫描图谱,确定母离子产生的丰度最高的特征子离子,以此对应的离子对及其比例对化合物进行定性分析,分别得到7种羟基多氯联苯衍生物的一级、二级质谱图,通过串联质谱法对每种目标化合物进行定量分析,仪器检出限范围为0.02-0.14μg/L,定量检出限为0.09-0.48μg/L。将本方法用于水产品中羟基多氯联苯的鉴别,结果满意。

Gaschromatography-tandemmassspectrometrywasadoptedtoidentifythehydroxylatedmetabolites of polychlorinated biphenyls and analyze the target compounds in fishery products. After the silylation derivatizaiton at 60 ℃ for 40 min, the MS spectrum of derivatives was obtained by GC/MS/MS under fullscan mode, and the fragment ions with the highest relative abundance were identified as m/z 399, 399, 399, 399, 399, 448 and 469, respectively which were defined as the precursor ion for product ion scan. The MS/MS spectrum was obtained under multiple reaction mode ( MRM ) by GC/MS/MS. And the product ions corresponded with the precursor ions were m/z 364, 364, 364, 364, 364, 433 and 434, respectively. The target compounds can be identified accurately by GC/MS/MS. In the present study, we took seven hydroxylated polychlorinated biphenyls as target compounds including 3-OH-PCB101 , 4-OH-PCB106 , 4-OH-PCB112 , 4''-OH-PCB101 , 3-OH-PCB118 , 3-OH-PCB138 and 3-OH-PCB180 . According to the iden

采用高效液相色谱-三重四级杆质谱(HPLC-MS/MS),对尿样中芥子气的小分子代谢产物硫二甘醇(TDG)、1-甲基亚砜-2-[2-(甲基硫醚)-乙基砜]乙烷(R6)和1,1’-砜-双[2-(甲基亚砜)乙烷](R7),进行一级质谱和二级质谱分析检测,建立了快速、高效、检测限更低的选择反应质谱检测(SRM)分析方法。该方法成功应用于禁止化学武器组织(OPCW)第二次生物医学样品演练未知尿样的分析检测,准确筛查出所有尿样中的芥子气小分子代谢产物。

Free metabolites of mustard gas contains thiodiglycol ,1-methylsulfinyl-2-[2-(methylthio )-ethylsulfonyl] ethane (R6) and 1 ,1''-sulfonyl-bis [2-(methylsulfinyl)ethane] (R7) .This article developed the method for analysis of the three free metabolites of mustard gas by HPLC-MS/MS .Using the method , we analyzed the unknown urine samples of the second confidence building exercise for biomedical sample a-nalysis from OPCW .The chemical components in the unknown urine samples were identified .

采用超高相液相色谱-三重四极杆串联质谱联用仪(UPLC-MS/MS),在电喷雾负离子模式下,对6个从西藏不同地区采集的大花红景天植物药材的甲醇提取液进行分析,通过准分子离子及其二级质谱碎片等信息归属了12个化合物,并且初步比较了样品中相关化合物相对含量的差异。结果表明,采集地不同,植物药材中化学组成存在明显的差异。

Six Rhodiola crenulata samples collected from different places in Tibet were extracted by methanol and analyzed using UPLC-ESI-MS/MS in negative-ion mode.In addition to 1 2 compounds iden-tified based on quasi-molecular ion and MS2 fragment ions,the differences of the relative content of relat-ed compounds were compared.The results showed that there were obvious differences in the composition of identified compounds in herbs with different collection places.

目的建立安神类中成药、保健食品中非法添加14种催眠类药物的定性和定量测定方法。方法使用RRLC-Q-TOF-MS作为检测方法,化合物准分子离子峰的保留时间、一级质谱和二级质谱作为定性依据;一级质谱准分子离子峰面积作为定量依据。结果建立安神类中成药、保健食品中非法添加14种催眠类药物的定性和定量检验测定方法,14种成分线性相关系数(r)均0.99,回收率80%~120%。结论 RRLC-Q-TOF-MS法定性准确,干扰少,定量线性及回收率良好,适用于安神类中成药、保健食品非法添加催眠类药品的定性和定量检验。

Objective To establish a qualitative and quantitative analysis method of illegally added 14 hypnotic drugs in Chinese traditional patent medicine and healthy foods. Methods RRLC-Q-TOF-NS was as the detection method. The qualitative analysis was based on the retention time,ms spectrometer and ms/ms spectrometer. The quantitative analysis was based on the quasi-molecular ion peak areas of 14 hypnotic drugs. Results The related coefficients of 14 components were all above 0. 99,the recover factors were between 80% ~120%. The qualitative and quantitative analysis method of illegally added 14 hypnotic drugs in Chinese traditional patent medicine and healthy foods was established. Conclusion This method is accu-rate and less interference,the liner relationships and the recover factors of the quantitative results are all well,which is suitable for the analysis of illegally added 14 hypnotic drugs in Chinese traditional patent medicine and healthy foods.