CAJ | 학술논문

为了建立高效、准确检测烟草总茄尼醇的方法,研究了超声辅助条件下,同步提取、皂化烟草茄尼醇的溶剂、温度、液料比、皂化剂用量、提取时间及超高效液相色谱测定的仪器条件.结果表明,烟草样品以正己烷为萃取剂,液料比为50:1, 0.1 moL/L氢氧化钠的乙醇溶液为皂化剂,在超声频率45 kHz,恒温水浴40℃,提取时间30 min条件下,完成烟草茄尼醇的提取、皂化,且使茄尼醇的提取、皂化以及与皂化剂的分离在同一离心管中完成.以ACQUITY UPLC BEH C18为色谱柱,甲醇-乙腈(50:50)为流动相,流速为0.5 mL/min,柱温为35℃,在波长208 nm条件下,超高效液相色谱进行检测.方法的线性范围为0.67~84.1 mg/L,方法检出限为0.07 mg/L,定量限为0.012%,空白及样品加标回收率分别在97.9%~104.7%、93.4%~102.3%范围内,相对标准偏差为 1.34%~2.43%.该方法简便、快速,且节约有机溶剂,精密度和准确度较高,可以实现烟草茄尼醇批量高效检测.
위료건립고효、준학검측연초총가니순적방법,연구료초성보조조건하,동보제취、조화연초가니순적용제、온도、액료비、조화제용량、제취시간급초고효액상색보측정적의기조건.결과표명,연초양품이정기완위췌취제,액료비위50:1, 0.1 moL/L경양화납적을순용액위조화제,재초성빈솔45 kHz,항온수욕40℃,제취시간30 min조건하,완성연초가니순적제취、조화,차사가니순적제취、조화이급여조화제적분리재동일리심관중완성.이ACQUITY UPLC BEH C18위색보주,갑순-을정(50:50)위류동상,류속위0.5 mL/min,주온위35℃,재파장208 nm조건하,초고효액상색보진행검측.방법적선성범위위0.67~84.1 mg/L,방법검출한위0.07 mg/L,정량한위0.012%,공백급양품가표회수솔분별재97.9%~104.7%、93.4%~102.3%범위내,상대표준편차위 1.34%~2.43%.해방법간편、쾌속,차절약유궤용제,정밀도화준학도교고,가이실현연초가니순비량고효검측.
In order to established the method of determining total solanesol in tobacco efficiently and accurately ,we studied the conditions of simultaneously extracting and saponifying solanesol from tobacco, including solvent, temperature, liquid ratio, saponification dosage, extraction time and ultrasound-assisted instruments conditions of ultra-high performance liquid chromatography. Hexane was used as solvent for extraction with liquid-material ratio of 50:1 and 0.1 moL/L sodium hydroxide in ethanol solution was used as saponification agent. The ultrasonic frequency used was 45 kHz, temperature of extraction and saponification was 40℃, and time of extraction was 30 min. Under this condition, extracting and saponifying solanesol from tobacco were finished simultaneously, and saponification agent separation was done in the same centrifuge tube. The separation of target compound was performed on an ACQUITY UPLC BEH C18 column using methanol-acetonitrile (50:50) as mobile phase by gradient elution. Flow rate was set at 0.5 mL /min, column temperature was 35℃ and injection volume was 5μL. The quantitative wavelength of UV detector was set at 208 nm. The results indicated that the calibration curve was linear in the range o f 0.67-84.1 mg/L, the limit of detection (LOD, S/N=3) was 0.07 mg /L, and the limit of quantification (LOQ, S/N=10) was 0.012%. The standard addition recoveries of blanks and samples were 97.9%-104.7% and 93.4%-100.0%, respectively, with relative standard deviations (RSDs) of 1.34%-2.43%. The method was simple, rapid, precisive, accurate, and solvent saving, suitable for batch testing .