SPE-GC/MS 法分析鱼塘水中的5种农药

目的：建立鱼类中毒案件中鱼塘水5种农药的固相萃取（solid phase extraction,SPE）结合气相色谱－质谱联用仪（GC/MS）的检测方法。方法比较 Oasis HLB cartridge、Bond Elut C18和 SampliQ C183种固相萃取柱提取、净化鱼塘水中5种农药的提取回收率,并考察洗脱剂种类、洗脱剂用量对提取回收率的影响。结果利用 Bond Elut C18固相萃取柱,以3mL 苯作为洗脱剂,鱼塘水中5种农药质量浓度在1~50μg/mL范围内有良好的线性关系,相关系数为0．9962~0．9996,测得的检出限为3．4~26μg/L,提取回收率为61．49%~102．48%,相对标准偏差均≤3．01%。结论 SPE－GC/MS 法灵敏度高、准确度和精密度好,简单快速,溶剂消耗量少,适用于鱼塘水中5种农药的检测。     

快速溶剂萃取-气相色谱-质谱联用法分析血液中的农药

目的：建立生物检材血液中农药的快速溶剂萃取（accelerated solvent extraction,ASE）法。方法通过优化ASE萃取条件,考察萃取温度、时间和萃取剂对回收率的影响,提取血液中的农药进行气相色谱-质谱联用（GC/MS）法定性定量分析。结果血液中8种农药的平均回收率在70.6%~92.4%,变异系数小于5.0%,8种农药在0.5~5.0μg/mL的浓度范围内线性良好。结论该方法具有操作简便快捷、回收率高、重现性好等特点,可用于农药的提取检验。     

超高效液相色谱-四极杆/静电场轨道阱高分辨质谱法检测血斑中乙醇生物标志物

Objective To establish a method for determination of two alcohol biomarkers (ethyl glucuronide, EtG;ethyl sulphate, EtS) in bloodstains via ultra-high performance liquid chromatography-quadrupole/electrostatic field orbitrap high-resolution mass spectrometry (UPLC-Q/eOrbitrap HRMS). Methods The bloodstains were prepared on clean glass slide where to have dropped the venous blood spiked of EtG or EtS, having them extracted with 50% hydrated methanol. The bloodstain-extracted supernatant was separated on a Synicronis C18 column (150mm×2.1mm×5.0μm) with gradient elution that was run through the mobile phases consisting of 0.1% formic acid (phase A) and acetonitrile: methanol (v/v 1:1) (containing 0.1% formic acid ) (phase B). MS tests were coupled with HPLC under HESI (heating electrospray ionization) source operated in negative ionization full-scan mode. Results Both EtG and EtS were linear with their calibration curves among the range of 0.2-100ng/patch (R²=0.9991, 0.9994), showing good recovery, intra-and inter-day precision less than 15%. The matrix effect was in the range of 85%-120%. Conclusion The method is effective to detect alcohol biomarkers (EtG and EtS) in bloodstains. © 2021, Editorial Office of Forensic Science and Technology. All rights reserved.     

ASE-GC/MS法检测血液中的常见镇静安眠类药物

目的建立ASE-GC/MS技术检测血液中常见镇静安眠类药物的方法。方法采用快速溶剂萃取(ASE)技术,对巴比妥、烯丙异丙巴比妥、异戊巴比妥、速可眠、SKF525、异丙嗪、去氧安定、氯丙嗪、利眠宁等9种镇静安眠类药物萃取后进行GC/MS检测,并对实验条件进行优化。结果经用ASE-GC/MS法检测空白添加血样,9种药物均获得很好的分离和检出。最佳萃取温度为110℃,萃取时间为3min,萃取溶剂为苯。9种药物在0.5~5.0μg/mL范围内线性关系良好,相关系数在0.984 2~0.998 1之间,检出限在1.0μg/mL左右。回收率在80.1%~106.3%之间,变异系数(CV)均小于3.62%。结论本文方法操作简便、快捷,回收率高,可用于常见镇静安眠类药物的检测。     

快速溶剂萃取-气相色谱/质谱法分析血液中的4种滥用药物

目的 建立生物检材血液中滥用药物的快速溶剂萃取（ASE）方法.方法 通过优化快速溶剂萃取各参数,提取血液中的滥用药物进行GC/MS定性定量分析.结果 血液中美沙酮、可卡因、蒂巴因、海洛因4种滥用药物的平均回收率在87.8％～97.5％之间,滥用药物在0.4μg/mL～4.0μg/mL的浓度范围内线性良好.结论 该方法具有操作简便快捷,回收率高、重现性好等特点,可广泛应用于生物检材血液中滥用药物的检验鉴定.