Weight Variation of Dietary Supplements

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1.0 Purpose 
 
 The purpose of this procedure is to provide instruction for the measurement of weight variation
 
 in all tableted, encapsulated, or chewable gel products that require weight variation at Ion Labs.
 
 2.0 Scope 
 
 This procedure applies to all tableted, encapsulated, or chewable gel products manufactured at
 Ion Labs, Inc. 
 
 3.0 Responsibility 
 
 3.1 It is the responsibility of trained QC personnel to follow this procedure.
 
 3.2 It is the responsibility of QC Laboratory Management to implement this procedure and
 
 keep procedure updated with current practices. 
 
 ee It is the responsibility of QC Laboratory Management to ensure that the procedure is
 
 followed. 
 
 4.0 Definitions 
 
 4.1 SD — Standard Deviation 
 
 4.2 RSD — Standard Deviation expressed as a percentage of the mean 
 
 4.3 Chewable Gel — Gummy vitamin product. 
 
 44 QC — Quality Control 
 
 
 

[SOP 

 Standard Operating Procedure SOP No Rev 
 D-712 Page 2 of 6 
 Weight Variation of Dietary Supplements 
 
 5.0 References 
 
 5.1 D-707, SOP, Use of Balances in the QC Laboratory 
 
 5.2. D-712-F1, Form, Weight Variation Form 
 
 5.3 USP <2091> Weight Variation of Dietary Supplements 
 
 6.0 Procedure 
 
 Note: This procedure requires an understanding of SOP D-707 Use of Balances in the QC
 Laboratory. 
 
 6.1 Equipment 
 
 6.1.1 Analytical balance with printer 
 
 6.2. Measuring weight variation in uncoated tablets 
 
 6.2.1 Weigh individually 20 whole tablets and calculate the average weight.
 
 6.2.2 Acceptance criteria: The requirements are met if the weights of not more than 2
 of the tablets differ from the average weight by more than the percentage listed in
 
 Table 1, and there is no tablet that differs in weight by more than double the
 
 percentage, unless otherwise stated in product profile. 
 
 6.3 Measuring weight variation in coated tablets 
 
 6.3.1 Weigh individually 20 whole tablets and calculate the average weight.
 
 6.3.2 Acceptance criteria: The requirements are met if the weights of not more than two
 
 of the tablets differ from the average weight by more than the percentage listed in
 Table 1, and there is no tablet that differs in weight by more than double that
 
 percentage, unless otherwise stated in product profile. 
 
 6.3.3. If the coated tablets do not conform to the criteria, place 20 tablets in 37°C
 
 Millipore water and gently swirl for up to 5 minutes. Repeat for a shorter period
 
 

[SOP 

 Standard Operating Procedure SOP No | Rev 
 D-712 8 Page 3 of 6 
 Weight Variation of Dietary Supplements 
 
 if any core disintegration has begun. 
 
 6.3.4 Dry un-disintegrated cores at 50°C for 30 minutes. 
 
 6.3.5 Weigh the 20 cores individually and calculate the average weight.
 
 6.3.6 Determine if the requirements meet the acceptance criteria. 
 
 6.3.7 In place of removing the coating from tablets, a representative sample of uncoated
 tablets from the corresponding batch can be used to assess weight variation.
 
 Formulation Weight of Tablet Acceptance % Difference 
 Measured 
 130mg or less 
 10 
 130mg — 324mg 
 70 
 324mg + 
 5 
 Table 1 Weight Variation Tolerances for Uncoated and Coated Tablets, unless otherwise stated
 in product profile 
 
 6.4 Measuring weight variation in Hard Capsules 
 
 6.4.1 Weigh individually 20 whole capsules and calculate the average weight.
 
 6.4.2 Acceptance Criteria: The requirements are met if each of the individual weights
 
 is within the limits of 90% and 110% of the average weight. 
 
 6.4.3 If not all of the capsules fall within the Acceptance Criteria uniquely identify 20
 capsules and weigh them individually documenting the weight with the capsule
 
 identifier. 
 
 6.4.4 Remove the contents of each capsule with the aid of a small brush or cotton swab.
 
 6.4.5 Weigh the identified shell and subtract the shell weight from the corresponding
 gross weight. 
 
 6.4.6 Calculate the average fill weight per capsule. 
 
 

[SOP 

 Standard Operating Procedure SOP No | Rev er 
 Weight Variation of Dietary Supplements D-712 8 8 
 
 6.4.7 The requirements are met if not more than two of the net weight differences are
 greater than 10% of the average net content and in no case is the difference greater
 
 than 25%, unless otherwise stated in product profile. 
 
 6.4.7.1 Ifthe requirements are not met because more than two but not more than
 
 6 capsules deviate from the average between 10% and 25%, determine
 
 the net contents of an additional 40 capsules. 
 
 6.4.7.2 Combine the original net data for the first 20 capsules with the additional
 
 40 capsules for a total of 60 capsules and calculate the net weight mean.
 
 6.4.7.3 The requirements are met if not more than 6 of the 60 capsules exceed
 
 10% of the average net content and in no case does the difference exceed
 25%. 
 
 6.5 Measuring Weight Variation in Soft Capsules 
 
 6.5.1 Proceed as directed in Section 6.4 Hard Capsules. 
 
 6.5.2 Ifthe soft capsules do not meet the Acceptance Criteria then uniquely identify 20
 soft capsules and weigh them individually documenting the weight with the soft
 
 capsule unique identifier. 
 
 6.5.3 Cut open the capsules by means of a suitable clean, dry cutting instrument such
 as scissors or a sharp open blade and remove the contents by washing with a
 
 suitable solvent. 
 
 6.5.4 Allow the occluded solvent to evaporate from the shells at room temperature over
 
 a period of no less than 30 minutes, taking precautions to avoid uptake or loss of
 moisture. 
 
 6.5.5 Continue evaluation from Section 6.4 Hard Capsules. 
 
 

[SOP 

 Standard Operating Procedure SOP No Rev ee 
 Weight Variation of Dietary Supplements D-712 8 8 
 
 6.6 Measuring Weight Variation of Chewable Gels 
 
 6.6.1 Weigh an equal number of units from each color and shape individually to obtain
 
 a total of NLT 20 individual weights, and calculate the average weight.
 
 6.6.2 The requirements are met if no individual weight differs from the average weight
 
 by more than 7.5%. 
 
 6.6.3 If 1 unit falls outside of the limits, repeat the procedure (6.6.1) with an additional
 
 set of NLT 20 chewable gels. The requirements are met if none of the units tested
 
 differ from the average weight by more than 10%. 
 
 6.7 Documenting Results 
 
 6.7.1 Only the official electronic form D-712-F1 Weight Variation may be used. All
 calculations will be performed using this electronic form which has all formulas.
 
 All Formulas are locked using a security passcode and the form traceable to user
 for modification and data entry. 
 
 6.7.2 The analyst will enter all weights into the electronic form. The form will be
 
 printed and taped into the laboratory notebook with the corresponding balance
 ticket. 
 
 6.7.3 The electronic form will be saved F:\Laboratory\Weight Variation Test in the
 correct folder for the year it was done. The file will be named with the Lot
 
 Number and Notebook Reference. 
 
 6.7.3.1 1.e. “240898 NB 318-95”. 240898 is the lot number and NB 318-95 is the
 
 notebook reference. 
 
 

[SOP 

 Standard Operating Procedure SOP No | Rev huehane 
 Weight Variation of Dietary Supplements oils $ : 
 
 7.0 Revision History 

| Rev | Date | Description of Changes | CCR # | By |
|-----|----------|------------------------|-------|----|
| 0 | 07/29/10 | New : ] 12/02/10 Updated SOP content : - | - | - |
| 2 | 03/31/11 | Updated SOP format - - | - | - |
| 3 | 02/21/13 | Updated with new format, updated forms to new format | 13-105 | B. Johns |
| 4 | 02/03/14 | Changed SOP title, removed HPLC test methods, added use of pre-coated tablets for assessment, clarified criteria on form. | 14-0120 | B. Johns |
| 5 | 09/16/16 | Biennial review: Updated format. Incorporated requirements of using electronic form including security requirements. Scheduled review: Updated responsibility and scope. Updated to Fae ; : shia include all forms of products produced at ION. piiaeteaaile an aia Added process for chewable gels. Updated form D-712-F1 to | 16-0825 | B. Johns |
| 7 | 09/30/22 | include a product type and dynamically acceptable adjust CC- ranges. Add “Unless otherwise stated in product profile” to sections | 22-0389 | J. Nicholson |
| 8 | 03/25/25 | hash hah eld CC- Removed Attachment and made Table 1 Updated Section 6.7 to reflect current practices | 25-0025 | M. Maples |