GB/T 22114-2021Humectants for toothpastes—Glycerin and polyethylene glycol (English PDF)

5.2 Test method for glycerin for toothpastes

5.2.1 Appearance

The test shall be carried out according to the provisions of GB/T 13216.

5.2.2 Odor

The test shall be carried out according to the provisions of GB/T 13216.

5.2.3 Color

The test shall be carried out according to the provisions of GB/T 13216.

5.2.4 Glycerin content

In the case of the simplified method, the test is carried out according to the density method (determination of glycerin content) in GB/T 13216; in the case of arbitration, the test is carried out according to the titration method (determination of glycerin content) in GB/T 13216.

5.2.5 Density

The test shall be carried out according to the provisions of GB/T 13216.

5.2.6 Chloride

The test shall be carried out according to the provisions of GB/T 13216.

5.2.7 Sulfated ash

The test shall be carried out according to the provisions of GB/T 13216.

5.2.8 Acidity or alkalinity

The test shall be carried out according to the provisions of GB/T 13216.

5.2.9 Saponification equivalent

The test shall be carried out according to the provisions of GB/T 13216.

5.2.10 Iron salts

The test is carried out according to method 0807 in the general rules of the Pharmacopoeia of the People's Republic of China 2015 edition (Volume IV).

5.2.11 Diethylene glycol and related compounds

5.2.11.1 Instruments

Gas chromatograph. it is equipped with a flame ionization detector; the chromatographic column is G43 [6% cyanopropyl phenyl - 94% p-methylpolysiloxane (mass fraction)] (0.53 mm×30 m×3 µm) elastic quartz capillary column, and the injection port liner type is an inward-rolled cup.

The chromatographic program is set as follows. the initial temperature of the chromatographic column is 100 °C. After injection, the temperature is increased to 220 °C at a rate of 7.5 °C/min and maintained for 4 min. The temperature of the injection port is maintained at 220 °C, and the temperature of the detector is maintained at 250 °C.

The carrier gas is helium. The split ratio is 10.1, and the column flow rate is 5 mL/min.

After the resolution liquid is injected, the chromatographic peak response is recorded according to the conditions specified in the determination method. The separation degree of the two peaks of diethylene glycol and glycerin in the chromatogram shall not be less than 7.0. Repeat the injection of the standard solution and record the chromatographic peak area. The relative standard deviation shall not exceed 15%.

5.2.11.2 Reagents

5.2.11.2.2 Resolution liquid

Accurately weigh chromatographically pure diethylene glycol and glycerin, dissolve them in water, dilute quantitatively, and dilute them stepwise with water when necessary to make solutions with a diethylene glycol and glycerin concentration of approximately 0.5 mg/mL.

5.2.11.2.3 Standard solution

Accurately weigh diethylene glycol, dissolve it in water, dilute it quantitatively, and dilute it step by step if necessary to make a solution with a diethylene glycol concentration of about 0.05 mg/mL.

5.2.11.2.4 Test solution

Accurately weigh 5.00 g of glycerin into a 100 mL volumetric flask, dissolve it in water and dilute to the mark, then shake well.

5.2.11.3 Test steps

According to the pharmaceutical excipients in the Pharmacopoeia of the People's Republic of China 2015 edition (Volume IV) and the corresponding labeled molecular weight of polyethylene glycol, the test shall be carried out according to the corresponding method for "ethylene oxide and dioxane" in the document.

5.3.7 Formaldehyde

According to the pharmaceutical excipients in the Pharmacopoeia of the People's Republic of China 2015 edition (Volume IV) and the corresponding labeled molecular weight of polyethylene glycol, the test shall be carried out according to the corresponding method for "formaldehyde" in the document.

5.3.8 Heavy metals

The test is carried out in accordance with the provisions of the first method of 0821 in the general rules of the Pharmacopoeia of the People's Republic of China 2015 edition (Volume IV).

5.3.9 Arsenic

The test is carried out in accordance with the provisions of the first method of 0822 in the general rules of the Pharmacopoeia of the People's Republic of China 2015 edition (Volume IV).

5.4 Net content

The net content of packaged humectants used for toothpaste shall be in accordance with the provisions of JJF 1070.

6.1 Classification of inspection

6.1.1 Factory inspection

The factory inspection items for glycerin include sensory indexes, physicochemical indexes, and requirements for diethylene glycol and related compounds.

The factory inspection items for polyethylene glycol include sensory indexes, physicochemical indexes, and requirements for toxic substance limit indexes.

6.1.2 Type inspection

All items specified in the technical requirements of this document are type inspection items. Under normal circumstances, a type inspection is carried out every three months. Type inspection shall be carried out in the following cases.

a) When key production processes are updated;

b) When there are changes in the main raw materials;

c) When production is resumed after suspension;

d) When the national quality supervision agency or the purchaser requests a type inspection.

6.1.3 Acceptance inspection

The purchaser has the right to inspect and accept the products received in accordance with the relevant terms of the contract signed by the supply and demand parties and the provisions of this document. The inspection and acceptance shall be completed within 15 days from the date of arrival of the goods.

6.2 Batching and sampling rules

6.2.1 Products of the same specifications delivered at one time are considered as one batch.

6.2.2 Products must first be inspected and certified by the quality inspection department of the manufacturer in accordance with the provisions of this document, and can only be shipped out after an inspection report is issued. The receiving unit shall accept and inspect in accordance with this document.

6.2.3 The sampling of glycerin and polyethylene glycol shall be carried out in accordance with GB/T 6678, GB/T 6679 and GB/T 6680, and the sampling volume shall not be less than 500 g.

6.3 Judgment rules

If the test results do not meet the standard requirements, re-sampling and re-testing shall be carried out. If the re-testing results still do not meet the requirements, the entire batch of products will be treated as unqualified products.

6.4 Sample storage and sample retention

Samples must be retained for each batch of accepted products and the samples shall be retained for 30 days.

7.1 Packaging

This product is a raw material for high-cleanliness oral hygiene and care products. The