Modification of Method for Rapid Determination of 3 Illicit Drugs in Human Urine by GC-MS with Pretreatment by DLLME
摘 要
对应用分散液液微萃取(DLLME)于气相色谱-质谱法(GC-MS)测定尿液中毒品的方法作了改进。分析时,在尿样2.0 mL中加入20.0 mg·L-1 SKF525A内标溶液100 μL,并调节其酸度至pH 12后,增加了加入N-丙基乙二胺(PSA)50 mg并振荡、离心的步骤,达到除去尿液中脂肪酸等杂质的目的,在后续操作中不会出现脂状沉淀。之后,取其上清液,加入分散剂异丙醇400 μL和萃取剂四氯化碳20 μL,轻轻振荡1 min并离心5 min后即可用微量移液器提取离心管尖底的小液滴1 μL,按GC-MS工作条件测定尿样中甲基苯丙胺、3,4-亚甲基二氧基苯丙胺(MDMA)和氯胺酮等3种毒品,其标准曲线的线性范围均在0.1~10.0 mg·L-1之间,检出限(3S/N)也相同,均为0.01 mg·L-1。试验测得3者的平均回收率依次为76.4%,83.2%,103%;三者测定值的相对标准偏差(n=5)依次为6.7%,5.3%,6.7%(日内)和7.5%,5.9%,6.6%(日间)。
Abstract
A modification for the dispersion liquid-liquid micro extraction (DLLME) in the sample pretreatment of rapid determination of 3 illicit drugs (i.e., methamphetamine, MDMA and ketamine) in human urine by GC-MS in hyphenation was proposed. In the analytical procedure, after the urine sample (2.0 mL) was mixed with 100 μL of 20.0 mg·L-1 internal standard solution of SKF525A, and its acidity was adjusted to pH 12, a modification of addition of 50 mg of PSA to the solution was made at this stage to remove impurities of fatty acid in urine, thus no precipitation of footy substance would happen in succeeding manipulations. After the addition of PSA, the mixture was centrifuged and the surpernatant was taken, to which 400 μL of iso-propyl alcohol (as dispersant) and 200 μL of CCl4 (as extractant) were added. The mixture was shocked lightly for 1 min and centrifuged for 5 min. 1 μL of the extractant (CCl4) at the shape bottom of the centrifuging tube was taken with a micropipet, and used for GC-MS determination of the 3 illicit drugs. Standard curves of the 3 drugs were found to have the same linearity range between 0.1 to 10.0 mg·L-1 and same detection limit (3S/N) of 0.01 mg·L-1. Test for recovery was made by standard addition method at 3 concentration levels, giving average recoveries of 76.4%, 83.2%, 103% for the 3 drugs respectively. Values of RSDs (n=5) found from the determined values of the 3 drugs were 6.7%, 5.3%, 6.7% (intraday) and 7.5%, 5.9%, 6.6% (interday) respectively.
中图分类号 O657.31 DOI 10.11973/lhjy-hx201912015
所属栏目 工作简报
基金项目
收稿日期 2019/5/27
修改稿日期
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备注刘缙,工程师,硕士,主要从事毒品毒物案件检验工作
引用该论文: LIU Jin,CAI Hongxin,QIAN Bin,DONG Wenbin,MAO Haifeng,LIANG Chen. Modification of Method for Rapid Determination of 3 Illicit Drugs in Human Urine by GC-MS with Pretreatment by DLLME[J]. Physical Testing and Chemical Analysis part B:Chemical Analysis, 2019, 55(12): 1442~1447
刘缙,蔡红新,钱斌,董文彬,毛海峰,梁晨. 分散液液微萃取预处理-气相色谱-质谱法快速测定人尿中3种毒品方法改进[J]. 理化检验-化学分册, 2019, 55(12): 1442~1447
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参考文献
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【2】张建华,黄颖,陈晓秋,等.分散液-液微萃取-高效液相色谱法测定环境水样中的多环芳烃[J].色谱, 2009,27(6):799-803.
【3】CUNHA R L, LOPES W A, PEREIRA P A P. Determination of free (unconjugated) amphetamine-type stimulants in urine samples by dispersive liquid-liquid microextraction and gas chromatography coupled to mass spectrometry (DLLME-GC-MS)[J]. Microchemical Journal, 2016,125:230-235.
【4】赵嘉祥,关雁飞,陈学国,等.离子液体-分散液液微萃取-高效液相色谱法测定尿中曲马多[C]//第四届全国“公共安全领域中的化学问题”学术研讨会论文集.中国辽宁沈阳, 2013:476-479.
【5】KIAROSTAMI V, ROUINI M R, MOHAMMADIAN R, et al. Binary solvents dispersive liquid-liquid microextraction (BS-DLLME) method for determination of tramadol in urine using high-performance liquid chromatography[J]. Daru-journal of Faculty of Pharmacy, 2014,22(1):25-25.
【6】MORADI M, YAMINI Y, BAHERI T. Analysis of abuse drugs in urine using surfactant-assisted dispersive liquid-liquid microextraction[J]. Journal of Separation Science, 2011,34(14):1722-1729.
【7】USUI K, HAYASHIZAKI Y, MINAGAWA T, et al. Rapid determination of disulfoton and its oxidative metabolites in human whole blood and urine using QuEChERS extraction and liquid chromatography-tandem mass spectrometry[J]. Legal Medicine, 2012,14(6):309-316.
【8】荣维广,阮华,吴建,等.QuEChERS法结合在线凝胶色谱-气相色谱/质谱法测定人体尿液中34种农药残留[J].中国食品卫生杂志, 2015,27(3):253-257.
【9】范茂林,杨旭东,艾雨,等.尿液中尼古丁和可替宁QuEChERS预处理气相色谱测定法建立[J].中国公共卫生, 2017,33(2):333-337.
【10】ANDRAŠĈÍKOVÁ M, HROUZKOVÁ S, CUNHA S C. Combination of QuEChERS and DLLME for GC-MS determination of pesticide residues in orange samples[J]. Food Additives and Contaminants: Part A, 2013,30(2):286-297.
【11】GARDNER M A, SAMPSEL S, JENKINS W W, et al. Analysis of fentanyl in urine by DLLME-GC-MS[J]. Journal of Analytical Toxicology, 2015,39(2):118-125.
【12】田海,郑尊涛,李建国,等.DLLME-GC测定水体中的毒死蜱和甲基对硫磷残留[J].农药, 2014,53(11):832-835.
【13】李明杰,张红医,刘晓哲,等.分散液-液微萃取萃取剂分散策略的新进展[J].分析化学, 2015,43(8):1231-1240.
【14】ITO R, USHIRO M, TAKAHASHI Y, et al. Improvement and validation the method using dispersive liquid-liquid microextraction with in situ derivatization followed by gas chromatography-mass spectrometry for determination of tricyclic antidepressants in human urine samples[J]. Journal of Chromatography B, 2011,879(31):3714-3720.
【15】徐梵姝,徐烨,刘丽华,等.DLLME-GC法同时测定尿样中4种芳烃类物质尿代产物[J].分析试验室, 2011,30(10):107-110.
【16】CELANO R, PICCINELLI A L, CAMPONE L, et al. Ultra-preconcentration and determination of selected pharmaceutical and personal care products in different water matrices by solid-phase extraction combined with dispersive liquid-liquid microextraction prior to ultra high pressure liquid chromatography tandem mass spectrometry analysis[J]. Journal of Chromatography A, 2014,1355:26-35.
【17】白宝清,王祺.盐析-涡旋辅助分散液液微萃取-液相色谱质谱联用法测定茶叶和果汁中有机磷农药残留[J].食品安全质量检测学报, 2017,8(3):935-941.
【18】GUPTA M K, JAIN R, SINGH P, et al. Determination of urinary PAH metabolites using DLLME hyphenated to injector port silylation and GC-MS-MS[J]. Journal of Analytical Toxicology, 2015,39(5):365-373.
【19】XIONG C M, RUAN J L, CAI Y L, et al. Extraction and determination of some psychotropic drugs in urine samples using dispersive liquid-liquid microextraction followed by high-performance liquid chromatography[J]. Journal of Pharmaceutical and Biomedical Analysis, 2009,49(2):572-578.
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