建立了全血中扎来普隆及其代谢产物5-氧扎来普隆和脱乙基扎来普隆超高效液相色谱-三重四级杆质谱(UPLC-TQ/MS)快速检验方法。采用改良后的QuEChERS前处理方法,全血样品用0.1%甲酸-乙腈提取,经无水MgSO4脱水净化,Waters BEH C18色谱柱分离,0.1%甲酸和0.1%甲酸-乙腈进行梯度洗脱。采用电喷雾电离,正离子(ESI+)模式扫描,多反应监测(MRM)模式检测。扎来普隆及其代谢产物在0.5~100 ng/mL范围内线性关系良好(R2≥0.997),回收率为92.0%~100.1%,相对标准偏差为1.9%~5.3%,方法检出限(S/N=3)均为0.05 ng/mL,定量限(S/N=10)在0.1~0.5 ng/mL范围内。
A fast testing method was established for the determination of zaleplon and its two metabolites, 5-oxozaleplon and desethylzaleplon, in blood by ultra performance liquid chromatography tandem electrospray ionization triple quadrapole-mass spectrometry (UPLC-TQ/MS). The optimized QuEChERS (Quick, Easy, Cheap, Effective, Rugged and Safe) method was used for sample preparation. The blood samples were extracted with 0.1% acetic acid and dehydrated by adding anhydrous magnesium sulfate. The targets were separated on a Waters BEH C18 column by gradient elution with 0.1% formic acid-0.1% formic acid/acetonitrile as mobile phase, ionized with positive electrospray (ESI+), and detected under multiple reaction monitoring (MRM) mode. As a result, zaleplon and its two metabolites displayed excellent linearity in the concentration of 0.5-100 ng/mL (R2>0.997). The average recoveries ranged from 92.0% to 100.1%. The RSD were in the range of 1.9%-5.3%. Besides, the limit of detection(LOD)of this method for target drugs was 0.05 ng/mL (S/N=3), while limits of quantification (LOQ) were in the range of 0.1-0.5 ng/mL (S/N=10). This method can meet the demand of rapidity and accuracy in the analysis of actual cases.
参考文献
| [1] | Gunja N. Journal of Medical Toxicology, 2013,9(2):155-162 |
| [2] | Moore K A, Zemrus T L, Ramcharitar V, Levine B, Fowler D R. Forensic Science International, 2003,134(2-3):120-122 |
| [3] | WEN Yu-Guan, MA Cui, QIU Chang, HOU Jing, LU Xin-Qiao. Pharmaceutical Journal of Chinese People’s Liberation Army, 2004,20(1):24-26 温预关, 马崔, 邱畅, 侯静, 陆欣乔.解放军药学学报, 2004,20(1):24-26 |
| [4] | Weitzel K W, Wickman J M, Augustin S G, Strom J G. Clinical Therapeutics, 2000,22(11):1254-1267 |
| [5] | Beer B, Ieni J R, Wu WH, Clody D, Amorusi P, Rose J, Mant T, Gaudreault J, Cato A, Stern W. J. Clin. Pharmacol., 1994,34(4):335-344 |
| [6] | ZHANG Lei-Ping, YU Zhong-Shan, HE Yi, CHANG Jing. Forensic Science and Technology, 2011,(1):13-15 张蕾萍, 于忠山, 何毅, 常靖.刑事技术, 2011,(1):13-15 |
| [7] | DENG Ming, ZHANG Su-Fen, LIU Jian-Fang, LIU Hui-Chen. Chinese Journal of Pharmaceutical Analysis, 2004,24(6):611-613 邓 鸣, 张素芬, 刘建芳, 刘会臣.药物分析杂志, 2004,24(6):611-613 |
| [8] | Karlonas N, Ramanavicius A, Ramanaviciene A. J. Sep. Sci., 2014,37(5):551-557 |
| [9] | Montenarh D, Hopf M, Maurer H H, Schmidt P, Ewald A H. Biotechnol. Pro., 2014,406(3):803-818 |
| [10] | ZHANG Lei-Ping, HUANG Shuang, SHU Cui-Xia. Forensic Science and Technolog, 2015,40(1):122-126 张蕾萍, 黄霜, 舒翠霞.刑事技术, 2015,40(1):122-126 |
| [11] | MA Ren-Ling, ZHOU Hong-Hua, LIU Wen-Hua, ZHANG Xi-Yue, FAN Yu. Journal of China Pharmaceutical University, 2003,34(4):330-333 马仁玲, 周红华, 刘文华, 张曦岳, 范瑜.中国药科大学学报, 2003,34(4):330-333 |
| [12] | Anastassiades M, Lehotay S J, Stajnbaher D, Schenck F J. J. AOAC Int., 2003,86(2):412-431 |
| [13] | LIU Man-Man, KANG Shu, YAO Cheng. Chinese Journal of Pesticide Science, 2013,15(1):8-22 刘满满, 康澍, 姚成.农药学学报, 2013,15(1):8-22 |
| [14] | DONG Mao-Feng, BAI Bing, TANG Hong-Xia, WANG Wei-Min, ZHAO Zhi-Hui, HAN Zheng, SONG Wei-Guo. Chinese J. Anal. Chem., 2015,43(5):663-668 董茂锋, 白冰, 唐红霞, 王伟民, 赵志辉, 韩铮, 宋卫国.分析化学, 2015,43(5):663-668 |
| [15] | ZHANG Chi, SONG Ying, PAN Jia-Rong, JIAO Bi-Ning, SUI Ke, LIANG Shi-Zheng, FENG Tao, FU Li-Li. Chinese J. Anal. Chem., 2015,43(8):1154-1161 张 弛, 宋莹, 潘家荣, 焦必宁, 睢珂, 梁世正, 冯涛, 付丽丽.分析化学, 2015,43(8):1154-1161 |
| [16] | LUO Yan-Bo, ZHENG Hao-Bo, JIANG Xing-Yi, LI Xue, ZHANG Hong-Fei, ZHU Feng-Peng, PANG Yong-Qiang, FENG Yu-Qi. Chinese J. Anal. Chem., 2015,43(10):1538-1544 罗彦波, 郑浩博, 姜兴益, 李雪, 张洪非, 朱风鹏, 庞永强, 冯钰锜.分析化学, 2015,43(10):1538-1544 |
| [17] | Usui K, Hayashizaki Y, Hashiyada M, Funayama M. Legal Med., 2012,14(6):286-296 |
| [18] | Lopes R P, Reyes R C, Romero-González R, Vidal J L, Frenich A G. J. Chromatogr. B, 2012,s895-s896(3):39-47 |
| [19] | WANG Peng, JIANG Xue-Hua, WANG Ling. Chinese Journal of New Drugs, 2011,(20):1953-1956 王 鹏, 蒋学华, 王凌.中国新药杂志, 2011,(20):1953-1956 |
| [20] | Lee S W, Choi J H, Cho S K, Yu H A, Abd EI-Aty A M, Shimb J H. J. Chromatogr. A, 2011,1218(28):4366-77 |
| [21] | Cajka T, Sandy C, Bachanova V, Drabova L, Kalachova K, Pulkrabova J, Hajslova J. Anal. Chim. Acta, 2012,743(18):51-60 |
| [22] | Ewa C, Anna S R, Ruiz J M M, Magdalena S Z. Food Chem., 2011,125(2):773-778 |
| [23] | YAO Meng-Kan, MA Bing-Liang, MA Yue-Ming. Chin. J. Pharm. Anal., 2010,30(12):2436-2439 姚梦侃, 马秉亮, 马越鸣.药物分析杂志, 2010,30(2):2436-2439 |
| [24] | Dmitrovic J, Chan S C, Chan S H Y. Toxicol. Lette., 2002,134(s 1-3):253-258 |
| [25] | GUO Zhen, CHANG Jing, YANG Rui-Qin, LUAN Yu-Jing, WANG Fang-Lin, YU Zhong-Shan. Journal of Instrumental Analysis, 2015,34(9):986-992 郭 震, 常靖, 杨瑞琴, 栾玉静, 王芳琳, 于忠山.分析测试学报, 2015,34(9):986-992 |
| [26] | Matuszewski B K, Constanzer M L, Chavez-Eng C M. Anal. Chem., 2003,75(13):3019-3030 |
- 下载量()
- 访问量()
- 您的评分：
-
10%
-
20%
-
30%
-
40%
-
50%