摘要
目的建立检测血液、尿液中阿片类毒品及其代谢物含量的气相色谱（GC）法或气-质联用（GC-MS）法。方法尿样或血样中的阿片类毒品,加0.1mol/mL（pH=6）磷酸缓冲溶液调节pH为5-6,将样品添加于固相萃取柱（SPE）,用去离子水和0.1mol/mL HCl淋洗,再次用CH3OH洗涤SPE柱子,由含2%氨水的CH2Cl2/CH3CH2OHCH3混合液萃取提取,吹干,用BSTFA＋TMCS（99∶1）试剂衍生化,以SKF-525a作为内标,利用色谱柱为DB-5MS的GC、GC-MS仪选择离子（m/z）扫描模式（SIM）和全扫描（Full Scan）模式进行测试分析。结果海洛因、吗啡、可待因、6-乙酰吗啡、6-乙酰可待因、乙基吗啡在25-400ng/mL范围内与峰面积呈良好的线性关系,相关系数r〉0.990 7,平均加内标回收率为95.9%-101.6%,相对标准误差（RSD）为2.13%-8.59%,最低检测限（LOD）为1ng/mL,最低定量限（LOQ）为25ng/mL。案件样品尿液检测出可待因、吗啡成分、6-乙酰吗啡成分,可待因含量〉400ng/mL,吗啡为384ng/mL,6-乙酰吗啡为278ng/mL,血液检测量极小,确证了吸食海洛因的违法事实。结论本方法简单、快速、灵敏度高、准确定性定量,适用于吸毒或毒品滥用者血样、尿样的筛查与确认试验。
Objective Establish gas chromatography（GC）and gas-mass spectrometry（GC-MS）methods to detect opioid drugs and their metabolites in the blood and urine.Methods Added pH6 phosphate buffer solution into urine or blood sample as 0.01 Mto adjust pH at 5-6,brought it into solid phase extraction column（SPE）,rinsed the column by deionized water and 0.01 M HCl,and then washed SPE column with CH_3 OH.Extracted by CH_2Cl_2/CH_3CH_2OHCH_3 mixture which were contained 2% ammonia and dried up,then derivatized with BSTFA＋TMCS（99∶1）reagent,took SKF-525 as internal standard,tested the content of the sample by DB-5 MS chromatographic column at ion（m/z）scan mode（SIM）and the full scan model of GC and GC-MS.Results There were good linear relationship between the contents of drugs（heroin,morphine,codeine,6-acetyl codeine,6-acetyl morphine,and ethyl morphine）and peak area in the range of 25-400μg/L,in which the correlation coefficient r was bigger than 0.9907;the average recovery rate of internal standard was 95.9-101.6%;the relative standard error（RSD）was 2.13%;the minimum limit of detection（LOD）was 1μg/L,the minimum limit of quantitative（LOQ）was 25μg/L.Codeine,morphine and 6-acetyl morphine in case urine sample could be detected.The content of codeine was〉400μg/L,morphine was 384μg/L,and 6-acetyl morphine was 278μg/L,while detection amount of blood samples were extremely low,but the illegal facts of heroin could be confirmed.Conclusion The methods were simple,rapid,high sensitivity and accurate quantitative and qualitative,which will be suitable for the screening and confirming test of blood and urine samples of drug addicters or drug abusers.
出处
《新疆医科大学学报》
CAS
2016年第7期849-853,857,共6页
Journal of Xinjiang Medical University
基金
新疆维吾尔自治区自然科学基金(201133132)
新疆维吾尔自治区乌鲁木齐市科技计划项目(Y111310019)
