RSC Advances
·
2023
·Vol. 13
·期 12
·7848-7856
·
IF 3.9
Hao Yang,Yinmeng Ding,Ya Ding,Jing Liu
Polycyclic aromatic hydrocarbons (PAHs) are a class of ubiquitous and persistent organic compounds that are significantly teratogenic, carcinogenic and mutagenic. Rubber stoppers commonly used in sterile formulation packaging materials often contain carbon black as the additive to enhance mechanical strength. However, PAHs may be formed during the production of carbon black, which could cause the drug formulations to be contaminated when contacting with the rubber stopper, and then enter the patient's body. The determination of PAHs in drug formulations is challenging, due to their trace amounts and matrix interference. Therefore, sample pretreatment is necessary and important. In this work, a novel technique, named in-vial solid-phase extraction (IVSPE), was developed for the selective extraction and enrichment of 16 PAHs in pharmaceuticals. The coated sample vial was directly used as the container for the whole process of sample pretreatment. As the solid-phase adsorbent, the coating was prepared by successively modifying the inner surface of a sample vial with polydopamine film and octadecylamine. PAHs could be selectively extracted through π–π stacking interaction and hydrophobic interaction, and then desorbed and enriched by a small amount of organic solvent. After systematic optimization of the coating preparation and the extraction process, the limits of detection and quantification of 16 PAHs were in the range of 0.002–0.60 ng mL−1 and 0.007–2.00 ng mL−1, respectively. Good linearities and precision of six repeated injections were obtained. The recoveries at three spiked concentration levels in normal saline were in the range of 62.72–106.90% with the relative standard deviation between 0.83% and 6.78%. Finally, PAHs in normal saline and powders for injection were extracted by established IVSPE, followed by separation and detection with high-performance liquid chromatography with a fluorescence detector and diode array detector (HPLC-FLD/DAD). It is worth noting that the preparation conditions of the adsorbent in the IVSPE method are mild, simple and green. Moreover, IVSPE has the advantages of having few work steps and avoiding the risk of contamination, because no special instrumentation or sample transfer is required. IVSPE could also be used for the pretreatment of multiple samples at the same time, which is beneficial to practical applications.
研究领域:
分析化学
·
药学
✓ 已验证
产品关联
DOI
PubMed
高影响因子
Current Pharmaceutical Analysis
·
2023
·Vol. 19
·期 4
·330-344
·
IF 0.6
Xu Bingyong,Gao Jiarui,Tang Kaixian,Zhang Fengmei,Liu Shan,Su Weike,Wang Jian
Background: To control the quality of various butyl rubber closures and assess their applicability to cefamandole nafate, HPLC/ GC-MS methods were developed to qualitatively and quantitatively analyze the organic components in various types of butyl rubber closures and drug powder of
cefamandole nafate for injection, and migration of these components from rubber closures to drug also were studied. Materials and Methods: The chemical components in the rubber closures and corresponding drug were identified by GC-MS in full scan mode and NIST mass library. A GC-MS method
in SIM mode was established to quantitatively analyze siloxane compounds, aromatic hydrocarbons and saturated chain-hydrocarbons in rubber closures and drugs. An HPLC method was established to quantitatively analyze antioxidants and sulfides from rubber closures and drugs. The turbidity values
of powder for injection were measured by a turbidimeter. Further, the correlation between the content of organic components in the drug and the clarity of the solution was analyzed. Results: It was found that the chemical components were released from butyl rubber closures and migrated
to the drug, which influenced solution clarity of cefamandole nafate for injection and was the main factor to cause solution turbidity of powder for injection. The gradual migration of components occurred over time with the use of common butyl rubber closures, but the coated butyl rubber closures
(rubber plated with membrane) were coated with a polytetrafluoroethylene film to block the contact between rubber closures and the drug, and could effectively prevent the migration of the components from rubber closures to drugs. The organic components in the butyl rubber closures were mainly
identified as siloxanes, saturated chain-hydrocarbons, and antioxidants. An unknown ingredient was identified as 1-piperidinecarboxaldehyde, and trace amounts of toxic toluene were also detected within limits. Conclusion: It is suggested that rubber plated with membrane or rubber closures
of high quality were applicable to cefamandole nafate for injection and should be used in its production. HPLC/ GC-MS methods can be used as an effective method for quality control of butyl rubber closures and compatibility research with drugs to ensure drug safety for the public.
研究领域:
药学
·
分析化学
✓ 已验证
DOI
高影响因子
Gels
·
2024
·Vol. 10
·期 10
·615
·
IF 5
Fan Yang,Fan Li,Renjing Ji,Xiaorong Yu,Huan Yang,Gaoshen Su
A self-degradable rubber plug (SDRP) was developed to address issues in existing crosslinked polymer temporary plugging technology, such as poor self-degradation properties. The synthesis formula was optimized using response surface analysis, resulting in an optimized composition of the SDRP: 13 wt% monomer, 0.02 wt% initiator, 0.7 wt% crosslinker, and 1.8 wt% degradation catalyst. Under the condition of 70–120 °C, the SDRP was transformed from a liquid to a solid gel in 30–110 min; the degradation time was 3–10 days, and the viscosity of the completely degraded solution was lower than 20 mPa·s. At an injection volume of 1 PV SDPR, a breakthrough pressure of 8.34 MPa was achieved. The hydrolysis of the unstable crosslinker was found to have caused the breakage of the SDRP. Over time, the functional groups within the unstable crosslinker underwent hydrolysis due to the combined effects of temperature and the degradation catalyst. This process led to the disruption of crosslinking points, resulting in a gradual deterioration of the network structure. As a consequence, some immobile water was converted into free water. The mobility of water molecules increased until the plug was completely degraded into a viscous liquid. This study enriches the temporary plugging gel system.
研究领域:
材料科学
·
石油工程
✓ 已验证
产品关联
DOI
PubMed
高影响因子
AAPS PHARMSCITECH
·
2021
·Vol. 22
·期 1
·1-9
·
IF 3.246
Sun Xuechun,Zheng Xin,Tang Yan,Debrah Augustine Atta,Du Zhenxia
Biological activity and pharmacological efficacy of protein drugs may be affected by the compatibility between drug and packaging materials. The compatibility of rubber closures seal cap has become the focus of many studies due to its complicated formulation. Despite of the significance of the issue, currently, there is little available data about organic leachables in drugs which is also not comprehensive. Since the concentration of migrants in drug is usually low and the matrix is complicated, the establishment of overall profile of extractables is crucial for the characterization of leachables. Herein, the supercritical fluid extraction (SFE) method was used because of its great extraction capacity and efficiency for low to medium polar extractables in rubber stoppers. The SFE conditions were optimized by response surface methodology (RSM). Experimental results of the extract yield were close to the predicted values ( R 2 = 0.95). Then the extractables were qualitatively and quantitatively analyzed with ultrahigh performance liquid chromatography quadrupole time-of-flight mass spectrometry (UHPLC-QTOF MS). Finally, risk assessment was made by comparing predicted exposure with injection permitted daily exposure (pPDE) limit or threshold recommended by threshold of toxicological concern (TTC). The results showed that there are many extractables such as glyceride, fatty acids and derivatives, antioxidants, and degradation products. Among them degradation products were in the majority and content of 17 substances exceeded corresponding limits. Considering their unknown toxicology, more experiments are therefore needed to provide information on their toxicology and risk assessment. The study provides a reference for the compatibility of drugs, and quality supervision of pharmaceuticals packaging.
研究领域:
药学
·
分析化学
✓ 已验证
DOI
PubMed
高影响因子
危险品化学品经营许可证（带存储）