超高效液相色谱法测定人血清中去甲万古霉素的含量
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摘要
目的建立测定人血清中去甲万古霉素含量的超高效液相色谱法。方法以Waters ACQUITY UPLC BEH C_(18)(2.1 mm×50 mm,1.7μm)为色谱柱,流动相为磷酸二氢钾缓冲液(pH=3.2)-甲醇(88∶12,v/v),流速0.21 mL·min~(-1),柱温42℃,检测波长:236 nm。10%高氯酸沉淀蛋白,离心取上清液进样。结果去甲万古霉素在1.67～83.40μg·mL~(-1)与峰面积线性关系良好(r=0.9991),低、中、高浓度(4.17、25.02、66.72μg·m L~(-1))的提取回收率分别为(66.30±2.1)%、(72.22±1.0)%、(75.32±0.8)%;方法回收率分别为(102.5±5.4)%、(97.5±1.1)%、(101.7±1.8)%。日内及日间精密度均小于3%(n=5)。结论该检测方法操作简单、准确、灵敏,可用于血清中去甲万古霉素的监测。
Objective To establish a UPLC method for norvancomycin concentration detection in the human serum. Methods Norvancomycin was extracted by 10% perchloric acid and separated by a Waters ACQUITY UPLC BEH C_(18)(2.1 mm×50 mm, 1.7 μm) column. The mobile phase was monopotassium phosphate buffer(pH= 3.2)-methyl alcohol(88∶12, v/v). The flow rate was 0.21 mL·min~(-1), the column temperature was at 42℃and the detection wavelength was at 236 nm. Results The linear range was from 1.67 to 83.40 μg·m L~(-1), r =0.9991. The extract recovery of low, medium, and high concentrations was(66.30±2.1)%,(72.22±1.0)%, and(75.32±0.8)% while the method recovery was(102.5±5.4)%,(97.5±1.1)%, and(101.7±1.8)%, respectively. The intra-and inter-day RSD was less than 3%(n = 5). Conclusion This method is simple, accurate, precise and suitable for the monitoring serum concentration of norvancomycin.
Objective To establish a UPLC method for norvancomycin concentration detection in the human serum. Methods Norvancomycin was extracted by 10% perchloric acid and separated by a Waters ACQUITY UPLC BEH C_(18)(2.1 mm×50 mm, 1.7 μm) column. The mobile phase was monopotassium phosphate buffer(pH= 3.2)-methyl alcohol(88∶12, v/v). The flow rate was 0.21 mL·min~(-1), the column temperature was at 42℃and the detection wavelength was at 236 nm. Results The linear range was from 1.67 to 83.40 μg·m L~(-1), r =0.9991. The extract recovery of low, medium, and high concentrations was(66.30±2.1)%,(72.22±1.0)%, and(75.32±0.8)% while the method recovery was(102.5±5.4)%,(97.5±1.1)%, and(101.7±1.8)%, respectively. The intra-and inter-day RSD was less than 3%(n = 5). Conclusion This method is simple, accurate, precise and suitable for the monitoring serum concentration of norvancomycin.
引文
[1]姜敏,罗丽芳,戴聿明,等. HPLC法测定去甲万古霉素血清药物浓度[J].实用临床医学,2011,12(11):1-3.
[2]王佳庆,梅升辉. RP-HPLC法同时测定人体血清及脑脊液中万古霉素的含量[J].药品评价,2012,9(23):22-25.
[3]焦志铁,张树倩.血浆去甲万古霉素的浓度测定[J].医药导报,2008,27(12):1523-1525.
[4]崔艳丽,武峰. HPLC法同时快速测定万古霉素和去甲万古霉素的血药浓度[J].中国医院用药评价与分析,2011,11(10):920-922.
[5]范捷,郭志磊,于洋,等.高效液相色谱法测定万古霉素血药浓度[J].中国医院药学杂志,2012,32(19):1590-1592.
[6]Diana J,Visky D,Rotts E,et al. Development and validation of an improved method for the analysis of vancomycin by liquid chromatography selectivity of Reversed-phase colums towards vancomycin components[J]. Chromatogr A,2003,996(1-2):115-131.
[7]林秀丽,朱金平,费燕. HPLC法快速测定万古霉素和去甲万古霉素的血药浓度[J].中国临床药学杂志,2011,20(4):231-234.
[8]陈方亮,余翠琴,刘海燕,等. HPLC法测定人血清中万古霉素和去甲万古霉素浓度[J].海峡药学,2012,24(6):260-263.
[9]吴健,汪永忠,韩燕全,等. UPLC法测定人血清中去甲万古霉素的浓度[J].中国药房,2013,24(30):2822-2824.
[10]编撰专家组.万古霉素临床应用中国专家共识(2011版)[J].中国新药与临床杂志,2011,30(8):561-573.
[2]王佳庆,梅升辉. RP-HPLC法同时测定人体血清及脑脊液中万古霉素的含量[J].药品评价,2012,9(23):22-25.
[3]焦志铁,张树倩.血浆去甲万古霉素的浓度测定[J].医药导报,2008,27(12):1523-1525.
[4]崔艳丽,武峰. HPLC法同时快速测定万古霉素和去甲万古霉素的血药浓度[J].中国医院用药评价与分析,2011,11(10):920-922.
[5]范捷,郭志磊,于洋,等.高效液相色谱法测定万古霉素血药浓度[J].中国医院药学杂志,2012,32(19):1590-1592.
[6]Diana J,Visky D,Rotts E,et al. Development and validation of an improved method for the analysis of vancomycin by liquid chromatography selectivity of Reversed-phase colums towards vancomycin components[J]. Chromatogr A,2003,996(1-2):115-131.
[7]林秀丽,朱金平,费燕. HPLC法快速测定万古霉素和去甲万古霉素的血药浓度[J].中国临床药学杂志,2011,20(4):231-234.
[8]陈方亮,余翠琴,刘海燕,等. HPLC法测定人血清中万古霉素和去甲万古霉素浓度[J].海峡药学,2012,24(6):260-263.
[9]吴健,汪永忠,韩燕全,等. UPLC法测定人血清中去甲万古霉素的浓度[J].中国药房,2013,24(30):2822-2824.
[10]编撰专家组.万古霉素临床应用中国专家共识(2011版)[J].中国新药与临床杂志,2011,30(8):561-573.