Abstract:

Objective A DART-HRMS method was developed for the rapid detection of gamma-hydroxybutyric acid and fluoroacetate in suspect samples. Methods According to the morphology of the samples, direct injection or injection after aqueous solution immersion was adopted. 12 Dip-it Samplers was used for injection. The instrument parameter were optimized to obtain the sensitive and accurate determination for GHB and fluoroacetate．In the negative ion mode , high intensity of [M-H]- ions were observed in Full MS mode with the sample introduction rate of 0.4 mm/s and by utilization of high purityhelium gas at 400 ℃． Results That the LODs of GHB in water, cola, iced tea and milk were 0.1, 0.5, 0.5 , 0.1μg/mL respectively. The LODs of fluoroacetate in water, vinegar, soy sauce and rapeseed oil were 0.01, 2, 2, 0.1μg/mL separately. This could meet the requirements of forensic science laboratory for the detection of the non-biological samples. This screening method would show its outstanding advantages including fast response, high-throughput potential to detect GHB and fluoroacetate in suspected samples. Conclusion  Local forensic laboratory we reanalyzed to testify the utility of the method. In the cases with complex and diverse samples, the positive and negative samples could be quickly identified, which could also provide a reference for the pre-treatment steps and prevent the high concentration samples contaminating the GC-MS or LC-MS instruments.

Key words:

direct analysis in real time, high resolution mass spectrometry, GHB, fluoroacetate,  , rapid screening

摘要：

目的 建立了一种快速检测可疑检材中γ-羟丁酸（GHB）和氟乙酸盐的实时直接分析－高分辨质谱法。方法 样品根据其形态采用直接进样或水溶液浸泡提取离心直接进样的方法，使用12 Dip－it Samplers模式进样，在负离子模式下，以全扫描模式采集准分子离子峰进行快速筛查。离子化温度为 400 ℃，进样速度为 0.4  mm/s。结果 γ-羟丁酸在水、可乐、冰红茶和牛奶中的检出限分别为0.1、0.5、0.5、0.1 μg/mL；氟乙酸盐在水、醋、酱油和菜籽油中的检出限分别为0.01、2、2、0.1 μg/mL，均能满足法庭科学实验室检验非生物检材中毒物的需求。该方法样品前处理简单、分析速度快，能快速并高通量筛查可疑检材中γ-羟丁酸和氟乙酸盐成分。结论 本方法在检材纷繁复杂多样时，可快速甄别法庭科学实验室的阳性检材和阴性检材，并为之后准确定性的前处理步骤提供依据，且防止高浓度检材污染气质或液质联用仪。

关键词:

实时直接分析, 高分辨质谱, γ-羟丁酸, 氟乙酸盐, 法庭科学, 快速筛查