高效液相色谱串联质谱检测尿液3种硫酸化胆汁酸

陈建波,欧阳小峰,张建明,丁敏

doi:10.13718/j.cnki.xsxb.2014.11.011

西南师范大学学报(自然科学版)

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高效液相色谱串联质谱检测尿液3种硫酸化胆汁酸

陈建波,欧阳小峰,张建明,丁敏. 高效液相色谱串联质谱检测尿液3种硫酸化胆汁酸[J]. 西南师范大学学报(自然科学版), 2014, 39(11). doi: 10.13718/j.cnki.xsxb.2014.11.011

引用本文:

CHEN Jian-bo,OUYANG Xiao-feng,ZHANG Jian-ming,DING Min. On Determination of Three Sulfated Bile Acids in Urine by High Performance Liquid Chromatography-Tandem Mass Spectrometry[J]. Journal of Southwest China Normal University(Natural Science Edition), 2014, 39(11). doi: 10.13718/j.cnki.xsxb.2014.11.011

Citation:

CHEN Jian-bo,OUYANG Xiao-feng,ZHANG Jian-ming,DING Min. On Determination of Three Sulfated Bile Acids in Urine by High Performance Liquid Chromatography-Tandem Mass Spectrometry[J]. Journal of Southwest China Normal University(Natural Science Edition), 2014, 39(11). doi: 10.13718/j.cnki.xsxb.2014.11.011

高效液相色谱串联质谱检测尿液3种硫酸化胆汁酸

陈建波,欧阳小峰,张建明,丁敏

昆明金域医学检验所有限公司昆明市医学实验诊断技术中心,昆明,650214 ; 重庆医科大学检验医学院,重庆,400016

On Determination of Three Sulfated Bile Acids in Urine by High Performance Liquid Chromatography-Tandem Mass Spectrometry

CHEN Jian-bo,OUYANG Xiao-feng,ZHANG Jian-ming,DING Min

摘要: 尿液样本经过 OASIS HLB 固相萃取，Luna C18色谱柱分离，流动相 A 为0.1％甲酸和2 mmol／L 乙酸铵水溶液，流动相 B 为0.1％甲酸和2 mmol／L 乙酸铵乙腈溶液，梯度洗脱，质谱采用负离子多反应监测检测模式．硫酸化石胆酸（3S‐LCA）、硫酸化牛磺石胆酸（3S‐TLCA）和硫酸化甘氨石胆酸（3S‐GLCA）3种硫酸化胆汁酸得到完全分离，线性范围分别为9.7～998.0，9.0～1080.0，9.3～1123.3 ng／mL ，检测限均为5 ng ／mL ，日内精密度均小于4.0％，日间精密度均小于5.0％，回收率在89.4％～100.7％范围内．本方法准确、灵敏，适用于尿液中硫酸化胆汁酸水平的实验室研究和临床检测．
- 高效液相色谱 /
- 串联质谱 /
- 硫酸化胆汁酸 /
- 妊娠肝内胆汁淤积症
Abstract: Urine samples are extracted with OASIS HLB SPE .The separations of sulfated bile acids are a‐chieved on a Luna C18 column with mobile phase consist of A (0 .1% formic acid and 2 mmol/L ammonium acetate in water ) and B (0 .1% formic acid and 2 mmol/L ammonium acetate in acetonitrile) by gradient e‐lution .The detection has been performed by multiple reaction monitoring in negative ion mode .The assays are linear in the range 9 .7 - 998 .0 ng/mL ,9 .0 - 1080 .0 ng /mL ,9 .3 - 1123 .3 ng/mL for 3‐sulfated tauro‐lithocholic acid (3S‐TLCA) ,3‐sulfated lithocholic acid (3S‐LCA) and 3‐sulfated glycolithocholic acid (3S‐GLCA ) ,respectively .The detection limits are 5 ng/mL for three sulfated bile acids .The precisions for three sulfated bile acids are CVs < 4 .0% for within‐day and CVs < 5 .0% for between‐day .The average recoveries for three sulfated bile acids are ranged from 89 .4 - 100 .7% .We have developed an accurate and sensitive method for the determination of urine three sulfated bile acids ,which are suitable for the clinical and research practice .
- high performance liquid chromatography-tandem mass spectrometry，sulfated bile acids，intra-hepatic cholestasis of pregancy /

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高效液相色谱串联质谱检测尿液3种硫酸化胆汁酸

陈建波,欧阳小峰,张建明,丁敏

昆明金域医学检验所有限公司昆明市医学实验诊断技术中心,昆明,650214 ; 重庆医科大学检验医学院,重庆,400016

关键词:

摘要: 尿液样本经过 OASIS HLB 固相萃取，Luna C18色谱柱分离，流动相 A 为0.1％甲酸和2 mmol／L 乙酸铵水溶液，流动相 B 为0.1％甲酸和2 mmol／L 乙酸铵乙腈溶液，梯度洗脱，质谱采用负离子多反应监测检测模式．硫酸化石胆酸（3S‐LCA）、硫酸化牛磺石胆酸（3S‐TLCA）和硫酸化甘氨石胆酸（3S‐GLCA）3种硫酸化胆汁酸得到完全分离，线性范围分别为9.7～998.0，9.0～1080.0，9.3～1123.3 ng／mL ，检测限均为5 ng ／mL ，日内精密度均小于4.0％，日间精密度均小于5.0％，回收率在89.4％～100.7％范围内．本方法准确、灵敏，适用于尿液中硫酸化胆汁酸水平的实验室研究和临床检测．

English Abstract

On Determination of Three Sulfated Bile Acids in Urine by High Performance Liquid Chromatography-Tandem Mass Spectrometry

昆明金域医学检验所有限公司昆明市医学实验诊断技术中心,昆明,650214 ; 重庆医科大学检验医学院,重庆,400016

Keywords:

Abstract: Urine samples are extracted with OASIS HLB SPE .The separations of sulfated bile acids are a‐chieved on a Luna C18 column with mobile phase consist of A (0 .1% formic acid and 2 mmol/L ammonium acetate in water ) and B (0 .1% formic acid and 2 mmol/L ammonium acetate in acetonitrile) by gradient e‐lution .The detection has been performed by multiple reaction monitoring in negative ion mode .The assays are linear in the range 9 .7 - 998 .0 ng/mL ,9 .0 - 1080 .0 ng /mL ,9 .3 - 1123 .3 ng/mL for 3‐sulfated tauro‐lithocholic acid (3S‐TLCA) ,3‐sulfated lithocholic acid (3S‐LCA) and 3‐sulfated glycolithocholic acid (3S‐GLCA ) ,respectively .The detection limits are 5 ng/mL for three sulfated bile acids .The precisions for three sulfated bile acids are CVs < 4 .0% for within‐day and CVs < 5 .0% for between‐day .The average recoveries for three sulfated bile acids are ranged from 89 .4 - 100 .7% .We have developed an accurate and sensitive method for the determination of urine three sulfated bile acids ,which are suitable for the clinical and research practice .