化学研究与应用
化學研究與應用
화학연구여응용
CHEMICAL RESEARCH AND APPLICATION
2010年
4期
415-419
,共5页
王燕燕%孟品佳%王彦吉%王川%李燕京
王燕燕%孟品佳%王彥吉%王川%李燕京
왕연연%맹품가%왕언길%왕천%리연경
海洛因%唾液%SPE提取%GC/SIM-MS检测
海洛因%唾液%SPE提取%GC/SIM-MS檢測
해락인%타액%SPE제취%GC/SIM-MS검측
heroin%saliva%solid-phase extraction%GC/MS-SIM detection
本文首先考查了不同类型不同厂家的固相萃取柱的萃取效果,采用提取效果较好的50 mg/mL的Cleanscreen CSDAUL01混合型强阳离子固相萃取柱,对唾液中的吗啡、可待因、6-单乙酰吗啡等3种鸦片类毒品进行提取后,将提取液吹干;再经MBTFA衍生化后,进行GC/MS-SIM检测.以乙基吗啡为内标,3种毒品的线性相关系数均大于0.99,线性范围为10~1000 ng/mL,相对回收率分别为85%~110%、94%~107%和75%~92 %;相对标准偏差小于10%.3种毒品的检测限分别为2 ng/mL、1 ng/mL和2 ng/mL.该方法灵敏度高、重现性好、操作简便,可用于鸦片类毒品滥用者及中毒者唾液中的毒品及其代谢物的检测.
本文首先攷查瞭不同類型不同廠傢的固相萃取柱的萃取效果,採用提取效果較好的50 mg/mL的Cleanscreen CSDAUL01混閤型彊暘離子固相萃取柱,對唾液中的嗎啡、可待因、6-單乙酰嗎啡等3種鴉片類毒品進行提取後,將提取液吹榦;再經MBTFA衍生化後,進行GC/MS-SIM檢測.以乙基嗎啡為內標,3種毒品的線性相關繫數均大于0.99,線性範圍為10~1000 ng/mL,相對迴收率分彆為85%~110%、94%~107%和75%~92 %;相對標準偏差小于10%.3種毒品的檢測限分彆為2 ng/mL、1 ng/mL和2 ng/mL.該方法靈敏度高、重現性好、操作簡便,可用于鴉片類毒品濫用者及中毒者唾液中的毒品及其代謝物的檢測.
본문수선고사료불동류형불동엄가적고상췌취주적췌취효과,채용제취효과교호적50 mg/mL적Cleanscreen CSDAUL01혼합형강양리자고상췌취주,대타액중적마배、가대인、6-단을선마배등3충아편류독품진행제취후,장제취액취간;재경MBTFA연생화후,진행GC/MS-SIM검측.이을기마배위내표,3충독품적선성상관계수균대우0.99,선성범위위10~1000 ng/mL,상대회수솔분별위85%~110%、94%~107%화75%~92 %;상대표준편차소우10%.3충독품적검측한분별위2 ng/mL、1 ng/mL화2 ng/mL.해방법령민도고、중현성호、조작간편,가용우아편류독품람용자급중독자타액중적독품급기대사물적검측.
In this paper,some solid-phase extraction columns in different types and from different manufacturers were tested,the better one among them with mixed strong cation exchange column(50 mg/mL of Cleanscreen CSDAUL01) was chosen to extract morphine,codeine and 6-acetyl morphine which spiked in saliva.Using ethyl morphine as an internal standard,and the 3 opiates spiked in blank saliva were extracted using a solid-phase cartridge,followed by being derivatized with MBTFA,and analyzed directly by GC/MS in selected ion mode.The method was validated in the range 10~1000 ng/mL with the drug-spiked saliva,the reactor responded linearly over the studied range(R~2> 0.99 for the 3 drugs);The relative standard deviations(RSD) were less than 15%,the relative extraction recoveries were varying from 75% to 110%,and LODs were less than 2 ng/mL,which promised the perspective application of the method in detecting trace amount of opium in human saliva.