LC-MS/MS Determination of Sildenafil in Health Food with On-Line Solid Phase Extraction of Molecularly Imprinted Monolithic Column
摘 要
采用原位聚合法,以西地那非为模板分子,甲基丙烯酸月桂酯为功能单体,乙二醇二甲基丙烯酸酯为交联剂,二甲基甲酰胺和十二醇为致孔剂,偶氮二异丁腈为引发剂,在不锈钢柱中制备西地那非分子印迹整体柱,并以西地那非分子印迹整体柱为在线固相萃取柱。粉碎均匀的保健食品样品用乙腈超声萃取30 min,再以8 000 r·min-1转速离心5 min,取上清液,残渣用乙腈重复萃取2次,合并上清液,并氮吹至近干。残留物用乙腈溶解并定容至1.0 mL,经0.22 μm有机尼龙膜过滤,采用分子印迹整体柱在线固相萃取-液相色谱-串联质谱法测定滤液中西地那非的含量。以Zorbax SB C18色谱柱为固定相,以不同体积比的0.1%(体积分数)甲酸溶液和乙腈的混合液为流动相进行梯度洗脱,串联质谱分析中采用电喷雾离子源(正离子扫描)和多反应监测模式。西地那非的质量浓度在0.5~100.0 μg·L-1内与其对应的峰面积呈线性关系,检出限(3S/N)为0.15 μg·kg-1。以空白样品为基体进行加标回收试验,所得回收率为93.5%~99.7%,测定值的相对标准偏差(n=6)为0.80%~2.1%。
Abstract
A sildenafil molecularly imprinted monolithic column was prepared in a stainless steel tube mold by in situ polymerization with sildenafil as template molecule, lauryl methacrylate as functional monomer, ethylene glycol dimethacrylate as crosslinker, dimethylformamide and dodecanol as porogens, and azobisisobutyronitrile as the initiator. The sildenafil molecularly imprinted monolithic column was used as on-line solid phase extraction column. The health food sample of crushing uniform was extracted ultrasonically for 30 min with acetonitrile, and then centrifugated for 5 min at the speed of 8 000 r·min-1. The supernatant was taken and the residue was extracted twice with acetonitrile. The supernatant was combined and evaporated to near dryness by N2-blowing. The residue was dissolved and diluted to1.0 mL with acetonitrile. The above solution was filtered with 0.22 μm organic nylon film. LC-MS/MS was applied to the determination of sildenafil in the filtrate with on-line solid phase extraction of molecularly imprinted monolithic column. Zorbax SB C18 chromatographic column was used as stationary phase, and the mixture of 0.1% (φ) formic acid solution and acetonitrile mixed in different ratios was used as mobile phase in gradient elution. ESI+ and multi-reactions monitor mode were adopted in MS/MS. Linear relationship between values of peak area and mass concentration of sildenafil was kept in the range of 0.5-100.0 μg·L-1, with detection limit (3S/N) of 0.15 μg·kg-1. On the base of blank sample, test for recovery was made by standard addition method; values of recovery found were in the range of 93.5%-99.7%, with RSDs (n=6) of determined values in the range of 0.80%-2.1%.
中图分类号 O657.63 DOI 10.11973/lhjy-hx201911002
所属栏目 试验与研究
基金项目 江苏省科技厅自然科学基金(BK20161166)
收稿日期 2019/1/18
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备注孙婷婷,副教授,硕士,研究方向为化学制药及化工新材料,563983393@qq.com
引用该论文: SUN Tingting,XU Yunhui,ZHANG Xuemei,QI Juan. LC-MS/MS Determination of Sildenafil in Health Food with On-Line Solid Phase Extraction of Molecularly Imprinted Monolithic Column[J]. Physical Testing and Chemical Analysis part B:Chemical Analysis, 2019, 55(11): 1247~1253
孙婷婷,徐云慧,张雪梅,祁娟. 分子印迹整体柱在线固相萃取-液相色谱-串联质谱法测定保健食品中西地那非[J]. 理化检验-化学分册, 2019, 55(11): 1247~1253
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【5】闫芳,夏宇,李威,等.西地那非治疗肺动脉高压的疗效及安全性研究[J].中国临床药理学杂志, 2014,30(10):877-879.
【6】唐文豪,马潞林,罗康平,等.男性对西地那非、伐地那非和他达拉非认识的研究[J].临床药物治疗杂志, 2007,5(2):28-31.
【7】刘德风,朱积川,姜辉,等.国产枸橼酸西地那非治疗男性勃起功能障碍的安全性和有效性研究[J].中华男科学杂志, 2017,23(1):43-48.
【8】沈志武,唐宏兵,李群,等.高效液相色谱法测定保健食品中他达拉非、西地那非、伐地那非违禁药物含量[J].理化检验-化学分册, 2008,44(6):540-542.
【9】邓鲲鹏,罗卓雅,雷毅.补肾壮阳类健康产品中艾地那非的检测方法研究[J].中国药学杂志, 2011,46(18):1441-1444.
【10】李绍辉,吴寒秋,许秀丽,等.超高效液相色谱串联质谱法检测玛咖产品中非法添加西地那非[J].食品工业科技, 2016,37(11):310-313.
【11】张丽媛,颜琳琦,周明昊,等.高效液相色谱-串联质谱检测保健酒中非法添加物艾地那非[J].食品科学, 2016,37(14):198-202.
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【14】张伟,孙成贺,王绍艳,等.人参皂苷Re分子印迹整体柱的制备与吸附[J].精细化工, 2015,32(10):1102-1105.
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