# US 2017/0282156 A1 · Extraction and determination of residual organic solvents in pharmaceutical products by spme method using a new nanocomposite fiber

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- Number: US 2017/0282156 A1
- Document ID: US20170282156A1
- Status: Published application
- Kind: A1
- Application number: 15/484,133
- Filed: 2017-04-11
- Published: 2017-10-05
- Earliest claimed: 2016-04-09
- Inventors: Alireza Ghiasvand; Fatemeh Yazdankhah; Kolsoum Nouriasl; Somayeh Hajipour
- Web page: https://patentgrep.com/patent/US20170282156A1

## CPC

- B01J 20/28007: {with size in the range 1-100 nanometers, e.g. nanosized particles, nanofibers, nanotubes, nanowires or the like (carbon nanostructures B01J20/205)}
- B01J 20/22: comprising organic material
- B01J 20/28023: {Fibres or filaments (fibres or filaments in the form of membranes B01J20/28038; B01J20/28007 takes precedence)}
- B01J 20/3236: {containing metal, other than zeolites, e.g. oxides, hydroxides, sulphides or salts}
- B82Y 30/00: Nanotechnology for materials or surface science, e.g. nanocomposites
- C25B 11/081: the element being a noble metal
- C01B 2202/06: Multi-walled nanotubes
- B01J: CHEMICAL OR PHYSICAL PROCESSES, e.g. CATALYSIS OR COLLOID CHEMISTRY; THEIR RELEVANT APPARATUS
- B82Y: SPECIFIC USES OR APPLICATIONS OF NANOSTRUCTURES; MEASUREMENT OR ANALYSIS OF NANOSTRUCTURES; MANUFACTURE OR TREATMENT OF NANOSTRUCTURES
- C25B: ELECTROLYTIC OR ELECTROPHORETIC PROCESSES FOR THE PRODUCTION OF COMPOUNDS OR NON-METALS; APPARATUS THEREFOR (anodic or cathodic protection C23F13/00; single-crystal growth C30B)
- C01B: NON-METALLIC ELEMENTS; COMPOUNDS THEREOF; {METALLOIDS OR COMPOUNDS THEREOF NOT COVERED BY SUBCLASS C01C}

## Abstract

A stainless steel wire may be platinized using electrophoretic deposition (EPD) method and then may be coated by polyaniline/multiwalled carbon nanotube (PANI/MWCNT) nanocomposite by electrochemical polymerization (EP). The resulting fiber may be used for headspace solid-phase microextraction (HS-SPME) of residual solvents (benzene, toluene, ethylbenzene and xylene, BTEX) in commercial pharmaceutical drugs, followed by gas chromatography-flame ionization detection (GC-FID).

## Claims

### Claim 1

A method to synthesize polyaniline/multiwall carbon nanotube (PANI/MWCNT) nanocomposite comprising:
decanting MWCNT and aniline into an electrolyte solution to prepare a PANI/MWCNT nanocomposite sorbent;
coating a stainless-steel wire with platinum to create a substrate for coating the PANI/MWCNT nanocomposite sorbent thereon;
inserting the platinum coated stainless-steel wire into the electrolyte solution;
coating the platinum coated stainless-steel wire with the PANI/MWCNT nanocomposite sorbent by applying a voltage to the platinum coated stainless-steel wire.

### Claim 2 (depends on 1)

The method of claim 1, wherein the platinum coated stainless-steel wire inserted into the electrolyte solution is used as an anode, the method further comprising inserting another wire into the electrolyte solution as a cathode.

### Claim 3 (depends on 2)

The method of claim 2, wherein coating the platinum coated stainless-steel wire with the nanocomposite sorbent includes coating the platinum stainless-steel wire with the PANI-MWCNT nanocomposite sorbent by applying the voltage between the anode and the cathode to create a fiber.

### Claim 4 (depends on 3)

The method of claim 3, wherein decanting MWCNT and aniline into the electrolyte solution includes decanting 0.1 g MWCNT and 0.05 M aniline into 30 mL of 0.05 M SDS electrolyte solution inside a 40 mL SPME vial with an aluminum cap to prepare the nanocomposite sorbent.

### Claim 5 (depends on 4)

The method of claim 4, wherein the aniline is kept in darkness and distilled prior to reaction.

### Claim 6 (depends on 3)

The method of claim 3, wherein the applied voltage between anode and cathode is 1.4 V for 300 seconds.

### Claim 7 (depends on 3)

The method of claim 3, wherein the fiber is coupled to Gas Chromatography-Flame Ionization Detector (GC-FID).

### Claim 8 (depends on 1)

The method of claim 1, wherein coating the platinum coated stainless-steel wire with the PANI/MWCNT nanocomposite sorbent includes coating the platinum coated stainless-steel wire with the PANI/MWCNT nanocomposite sorbent while the anode is rotating at 200 rpm.

### Claim 9 (depends on 1)

The method of claim 1, wherein coating the stainless-steel wire with platinum includes coating the stainless-steel wire with platinum via a two-electrode technique in an electrolyte solution comprising 0.42 g K2PtCl6 and 0.2 g H3BO3 in 20 mL water.

### Claim 10 (depends on 9)

The method of claim 9, wherein the two-electrode technique includes using the stainless-steel wire as an anode and another stainless steel wire as a cathode in a platinum solution.

### Claim 11 (depends on 10)

The method of claim 10, wherein the platinum solution is ultra-sonicated for 10 min and added in a 25-mL container, which is used as an electrochemical cell in a water bath at 80° C.

### Claim 12 (depends on 11)

The method of claim 11, wherein a 1 mA current flows between the anode and cathode for 5 seconds.

### Claim 13 (depends on 12)

The method of claim 12, wherein the anode and cathode are at 2 cm distance from each other.

### Claim 14 (depends on 1)

The method of claim 1, further comprising heat-treating the PANI/MWCNT for approximately 1 hour at 200° C.

### Claim 15 (depends on 1)

The method of claim 1, wherein the sorbent is configured for microextraction of the organic solvents of Benzene-Toluene-Ethyl Benzene-Xylene (BTEX) in penicillin.