摘要
建立了血液与尿液中麻黄碱和秋水仙碱的高效液相色谱-质谱联用（HPLC-MS）的同时测定方法。血液与尿液样品经三氟乙酸-乙腈（1：99）溶液提取后，用Waters Oasis MCX固相萃取小柱进行净化，在XDB-C8柱上以甲醇-0．04％（体积分数）三氟乙酸（33＋67）为流动相，采用电喷雾电离（ESI）在选择离子监测（SIM）模式下测定。定量分析离子：麻黄碱（m／z）166[M＋H]^＋；秋水仙碱（m／z）400[M＋H]^＋。麻黄碱和秋水仙碱在4．0～1000．0和6．0～1000．0μg·L^-1范围内均呈线性关系，检出限分别为4．0和6．0μg·L^-1，回收率在81．0％～109．0％范围内，其日内精密度〈6．4％，日间精密度〈9．9％。
Method of simultaneous determination of ephedrine and calchicine in blood and urine by HPLC-MS in hyphenation was proposed. Ephedrine and colchicine in blood or urine sample were extracted with a mixture of trifluoroacetic acid and acetonitrile （1＋ 99）, purified the Waters Oasis MCX micro-column and separated on the XDB-C8 column, using a mixture of methanol and 0. 04% trifluoroacetic acid solution （33＋67） as mobile phase. Determination was made by using ESI and under the mode of SIM. The ions of quantitative analysis were., ephedrine （m/z） 166[M＋H]^＋, calchicine （m/z） 400[M＋H]^＋. Linearity were held in the ranges of 4. 0-1 000.0 μg·L^-1 （for ephedrine） and of 6. 0-1 000.0 μg·L^-1 （for calchicine）, with detection limits of 4. 0 μg·L^-1 and 6. 0 μg·L^-1 respectively. Recoveries obtained were in the range of 81.0%- 109.05 for both compounds. The intra-day RSD and inter-day RSD found were 〈6.4% and 〈9. 9% respectively.
出处
《理化检验（化学分册）》
CAS
CSCD
北大核心
2006年第10期790-792,806,共4页
Physical Testing and Chemical Analysis(Part B:Chemical Analysis)
