Determination and risk assessment of heavy metals and harmful elements residues in Niuhuang Qingwei Pills based on ICP-MS / 中国中药杂志

To achieve a comprehensive understanding of heavy metals and harmful elements residues in Niuhuang Qingwei Pills,49 samples from 18 manufactures were collected from 31 provinces in China.Risk assessment and control preparations were applied innovatively in evaluation of exogenous pollution in traditional Chinese Medicine.Determination methods for Pb,Cd,As,Hg and Cu were established by inductively coupled plasma mass spectrometry(ICP-MS).Based on the procedures including hazard identification,hazard characterization,exposure assessment and risk characterization,risk assessment was performed and residual limits for Pb,Cd,As,Hg and Cu in the drug were formulated.The results showed that the hazardous quotients(HQ) of the elements were decreased in the following order:Pb>As>Cu>Hg>Cd,and the total hazardous index(HI) of heavy metals and harmful elements in Niuhuang Qingwei Pills was above 1,implying health risk of the drug.Under the proposed limits,5 elements in the control preparation as well as Cd and Cu in the samples were within the limits range,but the excess rates of Pb,As and Hg in the samples were 12%,12% and 14%,respectively.For the first time,basic steps for risk assessment of Chinese patent medicine were established,which provided model and reference for risk assessment and limit formulation of other drugs.

Adulteration situation of ophiopogonis radix in niuhuang qingwei pills / 中国药学杂志

OBJECTIVE: To establish the detection method of Liriopes Radix in Niuhuang Qingwei pills to uncover the adulteration situation of Ophiopogonis Radix in Niuhuang Qingwei pills. METHODS: Liriopesides B and liriope muscari baily saponins C in Niuhuang Qingwei pills were analyzed by HPLC-MS-MS in MRM mode. RESULTS： In the 18 batches of Niuhuang Qingwei pills, liriopesides B and liriope muscari baily saponins C, the index compounds of Liriopes Radix, were detected in 15 batches of samples in the concentrations of 0.10-1.19 μg·g-1. CONCLUSION： The adulteration of Ophiopogonis Radix with Liriopes Radix should be paid more attention to.

Fingerprint Study and Primary Quality Evaluation of Niuhuang Qingwei Pills Based on UPLC and Reference Drug / 中国药学杂志

OBJECTIVE： To apply reference drug in the fingerprint study of Niuhuang qingwei pills, and perform primary evaluation of the quality grade of the samples. METHODS： Ultra performance liquid chromatography (UPLC) separation was performed on an AQUITY UPLC BEH C18 column with gradient elution using acetonitrile (containing 0.5% formic acid)-0.5% formic acid at a flow rate of 0.2 mL•min-1. The injection volume was 2 μL and the column temperature was maintained at 40 ℃. The detection wavelength was set at 254 nm. By comparing with reference substances and the reference herbal materials, characteristic peaks and their ascriptions were investigated. Using Niuhuang qingwei pills reference drug as the accompanying physical control, the similarities of the fingerprints of 49 batches of samples from 18 manufacturers were calculated, and the quality grades were evaluated. RESULTS： The similarities of all samples fell within the range of 0.76-0.98. The similarities of 49 samples were above 0.75 and met the second-grade limit. The similarity of 24 samples were above 0.90 and met the first-grade limit. CONCLUSION： The method is simple, accurate and rapid. It can be used for the quality control and grade evaluation of Niuhuang qingwei pills, which provides reference for the quality grade research of Chinese patent medicines.

Simultaneous Determination of 7 Components in Niuhuang Qingwei Pills by HPLC-wavelength Switching Method / 中国药房

OBJECTIVE： To develop a method for simultaneous determination of 7 components of Niuhuang qingwei pills as chlorogenic acid， geniposide， forsythoside A， narirutin， baicalin， ammonium glycyrrhetate， chrysophanol. METHODS： HPLC-wavelength switching method was adopted. The determination was performed on Agilent ZORBAX SB-C18 column with mobile phase consisted of acetonitrile （A）-0.1％ phosphoric acid （B） gradient elution at the flow rate of 1.0 mL/min. The detection wavelengths were set at 348 nm （chlorogenic acid）， 238 nm （geniposide）， 330 nm （forsythoside A）， 280 nm （narirutin and baicalin）， 237 nm （ammonium glycyrrhetate）， 254 nm （chrysophanol）. The column temperature was 30 ℃， and sample size was 10 μL. RESULTS： The linear ranges of chlorogenic acid， geniposide， forsythoside A， narirutin， baicalin， ammonium glycyrrhetate， chrysophanol were 0.011 67-0.233 4 μg （r＝0.999 4）， 0.042 91-0.858 1 μg （r＝0.999 4）， 0.125 0-2.500 μg （r＝0.999 9）， 0.118 0- 2.360 μg （r＝0.999 9）， 0.119 6-2.392 μg （r＝0.999 7）， 0.030 57-0.611 4 μg （r＝0.999 6）， 0.006 201-0.124 0 μg（r＝0.999 4）， respectively； the limits of quantitation were 1.167， 0.858， 1.250， 1.180， 1.196， 0.611， 0.620 μg/mL， respectively； RSDs of precision tests were 0.98％， 1.04％， 0.59％， 1.50％， 0.83％， 1.24％ and 1.32％ （n＝6）， respectively. RSDs of stability tests were 1.21％， 0.97％， 1.42％， 0.71％， 0.98％， 1.87％ and 1.63％ （n＝6， 12 h）， respectively. Average recoveries were 98.32％， 98.11％， 98.81％， 98.50％， 98.30％， 98.16％ and 97.83％， and the RSDs were 1.37％， 1.41％， 0.64％， 1.01％， 1.18％， 1.16％ and 1.16％ （n＝6）， respectively. CONCLUSIONS： Established method is easy and reproducible. It can be used for the quality control of Niuhuang qingwei pills.

Determination of Emodin and Chrysophanol in Niuhuang Qingwei Pills by HPLC / 中国中医药信息杂志

Objective To establish a quality standard of Niuhuang Qingwei Pills.Methods Hypersil C18 was used with methanol-0.1% Phosphoric acid as mobile phase.The flow rate was 1.0 mL/min,detective wavelength was 254 nm,column temperature was 30 ℃ and injection valume was 10 ?L.Results Emodin and chrysophanol showed a good linear relationship in the range of 0.04～1.60 ?g(r =0.999 9).The average recovery was 99.92%(RSD=0.6%).Conclusion The established method is simple,feasible and reproducible,and can be used for the quality control of Niuhuang Qingwei Pills.