色谱
色譜
색보
CHINESE JOURNAL OF CHROMATOGRAPHY
2015年
8期
897-901
,共5页
胡婷婷%曲晓宇%康明芹%宋清莲%杨璐%赵韫慧%张代辉
鬍婷婷%麯曉宇%康明芹%宋清蓮%楊璐%趙韞慧%張代輝
호정정%곡효우%강명근%송청련%양로%조운혜%장대휘
高效液相色谱-高分辨质谱%壮阳药物%保健品%快速筛查
高效液相色譜-高分辨質譜%壯暘藥物%保健品%快速篩查
고효액상색보-고분변질보%장양약물%보건품%쾌속사사
high performance liquid chromatography-high resolution mass spectrometry ( HPLC-HRMS)%anti-impotence preparations%health care products%rapid screening
采用高效液相色谱-四极杆/飞行时间质谱对中药保健品中红地那非、伐地那非、那红地那非、他达拉非、西地那非、豪莫西地那非、硫代艾地那非、伪伐地那非、羟基豪莫西地那非、育亨宾、达泊西汀等11种非法添加的壮阳类药物进行了快速筛查、确证和定性定量检测。样品经甲醇提取后,采用正离子扫描模式进行检测。结果表明,11种待测物的定量限除那红地那非为25.0 ng/mL外,其他10种壮阳类药物均为5.0 ng/mL,在5.0~200.0 ng/mL(那红地那非在25.0~500.0 ng/mL)范围内,线性相关性较好,相关系数均不小于0.9990。平均添加回收率为82.0%~105.9%,相对标准偏差为4.7%~16.5%。本方法利用准确质量数匹配和自建标准谱库,通过多级特征碎片离子的比对,实现快速筛查和确证,简单快速,结果可靠。
採用高效液相色譜-四極桿/飛行時間質譜對中藥保健品中紅地那非、伐地那非、那紅地那非、他達拉非、西地那非、豪莫西地那非、硫代艾地那非、偽伐地那非、羥基豪莫西地那非、育亨賓、達泊西汀等11種非法添加的壯暘類藥物進行瞭快速篩查、確證和定性定量檢測。樣品經甲醇提取後,採用正離子掃描模式進行檢測。結果錶明,11種待測物的定量限除那紅地那非為25.0 ng/mL外,其他10種壯暘類藥物均為5.0 ng/mL,在5.0~200.0 ng/mL(那紅地那非在25.0~500.0 ng/mL)範圍內,線性相關性較好,相關繫數均不小于0.9990。平均添加迴收率為82.0%~105.9%,相對標準偏差為4.7%~16.5%。本方法利用準確質量數匹配和自建標準譜庫,通過多級特徵碎片離子的比對,實現快速篩查和確證,簡單快速,結果可靠。
채용고효액상색보-사겁간/비행시간질보대중약보건품중홍지나비、벌지나비、나홍지나비、타체랍비、서지나비、호막서지나비、류대애지나비、위벌지나비、간기호막서지나비、육형빈、체박서정등11충비법첨가적장양류약물진행료쾌속사사、학증화정성정량검측。양품경갑순제취후,채용정리자소묘모식진행검측。결과표명,11충대측물적정량한제나홍지나비위25.0 ng/mL외,기타10충장양류약물균위5.0 ng/mL,재5.0~200.0 ng/mL(나홍지나비재25.0~500.0 ng/mL)범위내,선성상관성교호,상관계수균불소우0.9990。평균첨가회수솔위82.0%~105.9%,상대표준편차위4.7%~16.5%。본방법이용준학질량수필배화자건표준보고,통과다급특정쇄편리자적비대,실현쾌속사사화학증,간단쾌속,결과가고。
A method was established for rapid screening and quantifying 11 illegally added anti-impotence preparations( yohimbine,acetildenafil,nor-acetildenafil,homosildenafil,hydroxy-homosildenafil,sildenafil,vardenafil,thioaildenafil,tadalafil,pseudovardenafil,dapoxetine ) in health care products by high performance liquid chromatography-high resolution mass spec-trometry. The samples were extracted with methanol and analyzed by positive mode in the MS detection. The results showed that the limits of detection were 25. 0 ng/mLexcept for nor-acetil-denafil( 5. 0 ng/mL ),the linear ranges were 5. 0-200. 0 ng/mL except for nor-acetildenafil (25. 0-500. 0 ng/mL)with the correlation coefficients not less than 0. 999 0. The recoveries were in the range of 82. 0%-105. 9% with the relative standard deviations of 4. 7%-16. 5%. This method is accurate,simple and rapid,and can be used in rapid screening and quantitative anal-ysis of the 11 illegally added anti-impotence in health care products.