Heo Seok, Choi Ji Yeon, Yoo Geum Joo, Park Sung-Kwan, Baek Sun Young
Advanced Analysis Team, National Institute of Food and Drug Safety Evaluation, Ministry of Food and Drug Safety, Osong Health Technology Administration Complex, Cheongju-si, Cheongwoungcheongbuk-do, Republic of Korea.
Biomed Chromatogr. 2017 Apr;31(4). doi: 10.1002/bmc.3856. Epub 2016 Nov 6.
A sensitive and specific LC/MS/MS method was developed for the simultaneous analysis of 35 compounds used for treating hypertension as adulterants in dietary supplements. The method was validated for specificity, linearity, accuracy, precision, limit of detection, limit of quantitation, stability and recovery. The limit of detection and limit of quantitation ranged from 0.20 to 20.0 and 0.50 to 60.0 ng/g, respectively. The linearity was good (r > 0.999), with intra- and interday precision levels of 0.43-7.87% and 0.65-9.95% and the intra- and interday accuracies of 84.36-115.82% and 83.78-118.69%, respectively. The stability (relative standard deviation) was <14.75%. The mean recovery was 80.81-117.86% (relative standard deviation <10.00%). Ninety-seven commercial dietary supplements available in South Korea were analyzed. While none contained detectable amounts of the 35 antihypertensive compounds, the developed LC/MS/MS procedure can be used for routine analysis to monitor illegal adulteration in various forms of dietary supplements.
开发了一种灵敏且特异的液相色谱-串联质谱(LC/MS/MS)方法,用于同时分析作为膳食补充剂掺假物的35种用于治疗高血压的化合物。该方法在特异性、线性、准确度、精密度、检测限、定量限、稳定性和回收率方面进行了验证。检测限和定量限分别为0.20至20.0 ng/g和0.50至60.0 ng/g。线性良好(r>0.999),日内和日间精密度水平分别为0.43 - 7.87%和0.65 - 9.95%,日内和日间准确度分别为84.36 - 115.82%和83.78 - 118.69%。稳定性(相对标准偏差)<14.75%。平均回收率为80.81 - 117.86%(相对标准偏差<10.00%)。对韩国市场上97种市售膳食补充剂进行了分析。虽然这些产品均未检测到35种抗高血压化合物,但所开发的LC/MS/MS方法可用于常规分析,以监测各种形式膳食补充剂中的非法掺假情况。