摘要
取1.00 g模拟样品,加入3 mL乙腈和2 mL水,涡旋5 min,超声提取20 min,离心5 min。上清液过预先活化好的Qasis HLB固相萃取柱,用5 mL乙腈洗脱,洗脱液于40℃氮吹至近干。用1.00 mL乙腈溶解残渣,过0.22μm有机滤膜,滤液供液相色谱-三重四极杆质谱仪分析。26种芬太尼类新精神活性物质和2种前体物质在ZORBAX SB-C18色谱柱上用不同体积比的甲醇和含0.005 mol·L^(-1)乙酸铵的0.1%(体积分数)甲酸溶液的混合溶液进行梯度洗脱分离,以电喷雾离子源正离子模式电离,多反应监测模式检测。通过解析质谱图,确定了28种目标物的母离子和子离子,并按照结构将其分为5组,推断出各组物质形成稳定子离子的可能断裂机理。方法验证试验结果表明,28种目标物的质量分数均在10~100μg·kg^(-1)内与其对应的峰面积呈线性关系,检出限(3S/N)为0.012~2.320μg·kg^(-1),回收率为86.2%~99.4%,测定值的相对标准偏差(n=5)为1.6%~6.3%。
An aliquot(1.00g)of the simulated sample was taken,and 3mL of acetonitrile and 2mL of water were added.The mixture was vortexed for 5min,extracted for 20min by ultrasound,and centrifuged for 5min.The supernatant was passed through the pre-activated Qasis HLB solid phase extraction column,in which targets were eluted with 5mL of acetonitrile.The eluate was blown to near dryness by nitrogen at 40℃.The residue was dissolved with 1.00mL of acetonitrile,and filtered through a 0.22μm organic filter membrane.The filtrate was analyzed by liquid chromatograph-triple quadrupole mass spectrometer.Twenty-six new psychoactive substances of fentanyl and 2precursors were separated on ZORBAX SB-C18column by gradient elution with mixed solutions composed of methanol and 0.1%(volume fraction)formic acid solution containing 0.005mol·L^(-1) ammonium acetate at different volume ratios,ionized by electrospray ion source positive ion mode,and detected by multiple reaction monitoring mode.The parent ions and daughter ions of the 28targets were determined by analyzing the mass spectra,and the targets were divided into 5groups according to their structures,which possible fracture mechanism of each group of substances to form stabilized daughter ions was deduced.As found by the results of tests for method validation,linear relationships between values of the mass fraction and the corresponding peak area of the 28targets were kept in the range of 10-100μg·kg^(-1),with detection limits(3S/N)in the range of 0.012-2.320μg·kg^(-1).The recoveries were found in the range of 86.2%-99.4%,and RSDs(n=5)of the determined values ranged from 1.6%to 6.3%.
作者
张爱平
施锦辉
黄健
孙雪婷
黄伟
丛於冬
李男
候晋
ZHANG Aiping;SHI Jinhui;HUANG Jian;SUN Xueting;HUANG Wei;CONG Yudong;LI Nan;HOU Jin(Nantong Customs,Nantong226004,China;Rudong Customs,Nantong226499,China)
出处
《理化检验（化学分册）》
CAS
CSCD
北大核心
2023年第5期497-505,共9页
Physical Testing and Chemical Analysis(Part B:Chemical Analysis)
关键词
液相色谱-三重四极杆质谱法
定性分析
定量分析
芬太尼
新精神活性物质
前体物质
liquid chromatography-triple quadrupole mass spectrometry
qualitative analysis
quantitative analysis
fentanyl
new psychoactive substance
precursor
