CAJ | 학술논문

目的建立唾液中褪黑素(镇静催眠药)浓度的HPLC-MS/MS测定方法.方法唾液样品经碱化后,用二氯甲烷萃取,以伊托必利作内标进样.色谱柱用Sunfire C18,柱温35℃;流动相为0.1%甲酸水溶液-甲醇,梯度洗脱,流量为0.3 mL·min~(-1);质谱用ESI离子源.结果本方法的定量下限是5.48 pg·mL~(-1)(S/N＞10),线性范围为5.48～250.00 pg·mL~(-1)(γ2=0.9994);最低检测限为2 pg·mL~(-1)(S/N＞3);本方法的日内、日间RSD均小于15%,提取回收率约为60%.结论本研究建立的褪黑素唾液浓度的测定方法快速、准确、灵敏度高.
목적 건립타액중퇴흑소(진정최면약)농도적HPLC-MS/MS측정방법.방법 타액양품경감화후,용이록갑완췌취,이이탁필리작내표진양.색보주용Sunfire C18,주온35℃;류동상위0.1%갑산수용액-갑순,제도세탈,류량위0.3 mL·min~(-1);질보용ESI리자원.결과 본방법적정량하한시5.48 pg·mL~(-1)(S/N＞10),선성범위위5.48～250.00 pg·mL~(-1)(γ2=0.9994);최저검측한위2 pg·mL~(-1)(S/N＞3);본방법적일내、일간RSD균소우15%,제취회수솔약위60%.결론 본연구건립적퇴흑소타액농도적측정방법쾌속、준학、령민도고.
Objective To establish a HPLC-MS/MS method for the determination of melatonin in human saliva.Methods Sabra samples and internal standard(itopride)were extracted by dichloromethane after alkalization.The analysis was conducted using a Sunfire C18 column with gradient elution and the column temperature iS 35 ℃.The mobile phase consisted of methanol and water with 0.1%formic acid at flow rate of 0.3 mL·min~(-1).Analysis in mass Was operated by the electrospray ionization.Results LLOQ of the method is 5.48 pg·mL~(-1)(S/N ＞10).The standard curve is linear in the range of 5.48～250.00 pg·mL~(-1)(γ2=0.9994).LLOD is 2 pg·mL~(-1)(S/N＞3).The RSDs of interday and intra-day are all less than 15%.The extraction recovery is closed to 60%.Conclusion The method is fast,precise and sensitive,and suitable for the determination of melatonin in human saliva.