SPE-UHPLC-MS/MS Determination of 13 Forbidden Male-genito-function-Strengthening Drugs in Traditional Chinese Medicines and Health-care Food
摘 要
固样(2.000 0 g)加水10.0 mL使其超声分散(液样取2.00 mL,加水8.0 mL),加甲醇稀释至50.0 mL。取上清液2.00 mL,用0.1 mol·L-1盐酸溶液稀释至10.0 mL。所得溶液经Cleanert PCX混合型阳离子固相萃取柱净化、氨水-甲醇(5+95)混合液洗脱。洗出液进行色谱分离,用ZORBAX SB-C18色谱柱作固定相,并以不同体积比的乙腈和0.01 mol·L-1乙酸铵溶液(pH 3.5)的混合液为流动相进行梯度淋洗。质谱分析中,采用电喷雾正离子源和多反应监测模式检测。13种壮阳类化合物的质量浓度在1.0~1 000 μg·L-1范围内呈线性,方法的检出限(3S/N)在3.0~40 μg·kg-1之间。加标回收率为80.1%~111%,相对标准偏差(n=6)小于8%。
Abstract
Solid sample (2.000 0 g) was dispersed ultrasonically in 10.0 mL of water, or 2.00 mL of liquid sample was mixed with 8.0 mL of water, and then diluted to 50.0 mL with CH3OH. 2.00 mL of the supernatant was taken and diluted to 10.0 mL with 0.1 mol·L-1 HCl solution, and then purified by passing through Cleanert PCX mixed cationic SPE column, which was then eluted with a mixture of aq. ammonia and methanol (5+95). The eluate was separated on ZORBAX SB-C18 column using mixtures of 0.01 mol·L-1 NH4OAc solution (pH 3.5) and acetonitrile in various ratios as mobile phase in gradient elution. ESI+ and MRM were adopted in MS. Linear relationships between values of peak areas and mass concentrations of the 13 forbidden drugs were obtained in the same range of 1.0-1 000 μg·L-1, with values of detection limits (3S/N) in the range of 3.0-40 μg·kg-1. Tests for recovery were made by standard addition method, giving values of recovery in the range of 80.1%-111%, with values of RSDs (n=6) less than 8%.
中图分类号 O657.63 DOI 10.11973/lhjy-hx201701009
所属栏目 工作简报
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收稿日期 2016/1/13
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备注咸瑞卿(1981-),男,山东临沂人,主管药师,研究方向为食品保健品检测。
引用该论文: XIAN Rui-qing,SHI Feng,MU Wei-wei,WANG Xiao-bing,LI Qi-yan. SPE-UHPLC-MS/MS Determination of 13 Forbidden Male-genito-function-Strengthening Drugs in Traditional Chinese Medicines and Health-care Food[J]. Physical Testing and Chemical Analysis part B:Chemical Analysis, 2017, 53(1): 44~49
咸瑞卿,石峰,牟卫伟,王小兵,李启艳. 固相萃取-超高效液相色谱-串联质谱法测定中药和保健食品中13种禁用壮阳类药物含量[J]. 理化检验-化学分册, 2017, 53(1): 44~49
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【3】石岩,魏锋,朱晓鹏,等.中药及保健食品中PDE5抑制剂检测的再研究[J].药物分析杂志, 2014,34(1):121-129.
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【7】MAN C N, NOOR N M, LAJIS R. Identification of thioketone analogues of sildenfil using gas chromatography-mass spectrometry[J]. Journal of Chromatography A, 2011,1218(39):7055-7060.
【8】LI Yang, HU Jiang-tao, SHI Ying, et al. Simultaneous determination of seven adulterants in slimming functional foods by HPLC-ESI-MS/MS[J]. Food Anal Methods, 2011,4(4):505-516.
【9】SHI Feng, GUO Chang-chuan, GONG Li-ping, et al. Application of a high resolution benchtop quadrupole-orbitrap mass spectrometry for the rapid screening, confirmation and quantification of illegal adulterated phosphodiesterase-5 inhibitors in herbal medicines and dietary supplements[J]. Journal of Chromatography A, 2014,1344:91-98.
【10】PARK S R, LEE J G, ROH S H, et al. Determination of PDE-5 inhibitors and appetite suppressants in adulterated dietary supplements using LC/PDA and LC/MS[J]. Food Addit Contam Part B Surveill, 2012,5(1):29-32.
【11】李锦清,綦艳,郦明浩,等.超高效液相色谱-串联质谱法同时测定保健品中三种违禁成分[J].现代食品科技, 2014,30(11):246-250.
【12】苏萌,艾连峰.液相色谱-串联质谱基质效应及其消除方法[J].食品安全质量检测学报, 2014,5(2):511-515.
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